Document k97LdYDVwQgD9GnR9Oxr60qmb

Egen, _ Pecse Reseach '. Proven Results. Enclosure 5 -... AnalyticaRl eport Fluorochemical Characterization of Water and Sediment Samples Decatur Bakers Creek #2 - July 2003 (E03-0561) Exygen Research Laboratory Report No. L34910 Revision 1 Testing Laboratory i . Exygen Research 3058 Research Ddve State College, PA 16801 _ " Requester Jess Eldridge 3M Environmental Technology and Safety Services 935 Bush Avenue Building 0002-03-E-09 PO Box 33331 ST. Paul, MN 55t33-3331 "i V " _F'3058 h' IState PAGE ResearchDrive College,PA16801, USA 814.272.1019 ex_en.com I I I 1 Introduction Results are reported for the analysis of surface water and sediment samples received by E.xygen Research (Exygen) from Pace Analytical. The Exygen study number assigned to the project is L34910. Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC/MS/MS) was requested for all samples. A total of 26 samples were received for analysis. The samples were prepared and analyzed by LC/MS/MS for the following list of fluorochemicals: Table 1: Target Analysis Compound Name Acronym Perfluorohexanesulfon.ate C6 Sulfonate (PFHS_ Perfluorooctanesulfonate C8 Sulfonate (PFOS) 1 Perfluorooctanoic Acid Perfluorooctanesulfonylamide C8 Acid (PFOA) FOSA The analytical methods used were originally developed for groundwater samples and were _d' validated by Exygen. The validation protocol and results are on file with Exygen. Only the C8 Sulfonate, FOSA, and C8 Acid were included in the original method validation. It should be noted that the quality control elements included in this analysis demonstrate the applicability of the method to the additional analytes. 2 Sample Receipt The samples were submitted in plastic containers. All samples were cooled to 4C from time of collection to receipt at Exygen Research. Samples were stored at 4C from receipt at F__.xygen Research until analysis. Samples were collected on 7/21/03 and 7/23/03. Chain-of-custody information is presented in Attachment C. 3 Holding Times Field and laboratory spikes of these fluorochemicals have shown stability for periods greater than 90 days. Samples were analyzed within 30 days of receipt. V PAGE2OF5 I II tlf 4 Methods - Analytical and Preparatory 4.1 4.1.1 LC/MS/MS Sample Preparation for LC/MS/MS Analysis Water samples were initiallytreated with 200 uL of 250 mg/l_sodium thiosulfatesolution to remove residualchlorine.Solid phase extraction(SPE) was used to prepare the samplesfor LC/MS/MS analysis. A forty-millilitepr ortionof sample was used for analysis. The samples were transferredto a C18 SPE cartridge. The cartridgewas eluted with 5 mL of 100% methanol.This treatment resultedin an eight-foldconcentrationof the ditutedSamplespriorto analysis. Sediment samples were first extracted into methanol (5 grams of sediment to 5 mL of methanol). The methanol extract was diluted to forty-millilitersand treated in the same manner as the water samples, using SPE. 4.1.2 Sample Analysis by LCJMS/MS In HPLC, an aliquot of extract is injected and passed through a liquid-phase chromatographic ! column. Based on the affinity of the analyte for the stationary phase in the column relative to the liquidmobile phase, the analyte is retained for a characteristic amount of time. Following HPLC separation, ES/MS provides a rapid and accurate means for analyzing a wide range of organic compounds, including fluorochemicals. Electrospray is generally operated at relatively mild temperatures; molecules are ionized, fragmented, and detected. Ions characteristic of known fluorochemicals are observed and quantitated against standards. A Hewlett-Packard HP1100 HPLC system coupled to a Micromass UItima MS/MS was used to analyze the sample extracts. Analysis was performed using selected reaction monitoring (SRM). Samples extractions and analyses were performed between 7/31/03 and 8/13/03. Exact dates for extraction and analysis of each sample batch are given in the raw data. Raw analytical data is provided in Attachments D and E. 5 Analysis 5.1 Calibration A 7-pointcalibrationcurve was analyzedat the beginningand end of the analyticalsequence for the compoundsof interest.The calibrationpointswere prepared at 0, 25, 50, 100, 250, 500, and 1000 ng/L (ppt) for LC/MS/MS analysis. The instrument response versus the concentrationwas plottedfor each point. Using linearregressionwith 1/x weightingt,he slope, y-interceptand correlationcoefficient(r) and coefficientof determination(r=)were determined. A calibration curve is acceptableif r >0.985 (r2 _>0.970). Calibration standards are prepared using the same SPE procedure used for samples. Calibration check standards were analyzed periodically (every three to five sample injections) throughout the analysis sequence. Compliance is obtained if the standard analyte concentrations are within +/-20=/oof the actual value. V All calibration criteria were met for this analysis. PAGE 3 OF 5 V 5.2 Blanks Extractionblanks were prepared and analyzed with every extractionbatch of samples. The extractionblanksshouldnot have anytarget analytes presentat or above the concentrationof the low-levelcalibrationstandard. For thesesamples,theextractionblankswere compliant. Instrumentblanksin the form of clean methanol solventwere also analyzed after every highlevel calibrationstandard,and after knownhigh-levelsamples. Again, the blanks shouldnot have any target analytes present at or above the low-levelcalibration 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 analyticalmethods. 5.4 Matrix Spikes Field matrix spikes were prepared at low and high levels for each sample for all compounds of interest. Single laboratory matrix spikes were also performed for each sample. Laboratory control spikes (see section 5.6) consisting of laboratory water spiked at the time of extraction were performed with each analytical set. Matrix spike recoveries are given in Attachment B. 4 For sediment samples, recovery is calculated from the amount present in the sample extract. Please see Section 5.7 for additional discussionof matrix spike recoveries. 5.5 Duplicates Field and laboratoryduplicateswere performed for each sample. The duplicateresultsare includedwiththe sampleresultsin AttachmentA. 5.6 Laboratory Control Samples For LC/MS/MS analyses, Milliqwater was spikedwithall compoundswitheach extractionset. All recoveriesfor all compounds were between 70-130% in each LCS. Results are given along with the rawdata in Attachment D. 5.7 Statement of Accuracy Based on results of field spikes, laboratory spikes, field blank spikes, and laboratory control spikes, the analytical accuracy for all compounds is + 30%. Exceptions for the water samples are as follows: BC2 SW-04 high spike (PFOA - 57%, PFOS - 62%, FOSA - 58%); BC2 SW05 high spike (PFOA - 66%, FOSA - 40%), BC2 SW-06 high spike (FOSA - 60%), Outfall to River SW-25 (FOSA - 58%). Also, several low spike samples showed unacceptable recoveries in cases where the spiking concentration was comparable or below the inherent sample concentration. However, all laboratory control spikes, laboratory matrix spikes, and all other field spikes showed recoveries between 70% and 130% for all compounds. The accuracy for the sediment samples is based upon laboratory spike recoveries, all of which were between 70% and 130% for allcompounds. 6 Data Summary Please see Attachment A for a detailed listing of the analytical results. Results are reported in parts per billion (ppb) (ng/mL) for the water samples. Sediment samples are also reported in units of parts per billion (ppb) (ng/g). Sediment results are reported on both an as-received V and dry-weight basis. PAGE4OF5 q_ 7 Data Retention Samplesare disposedof onemonthafterthe reportisissuedunlessotherwisespecified.All electronicdata is archivedon retrievablemedia and hard copy reportsare stored in data foldersmaintainedby Exygen. 8 Attachments 8.1 AttachmenAt: Results 8.2 AttachmenBt :MatrixSpikeRecoveries 8.3 AttachmentC: Chainof Custody 8.4 AttachmentD: RawAnalyticalData(SurfaceWaterSamples) 8.5 AttachmentE: RawAnalyticalData(SedimenSt amples) 9 Signatures PaulConnolly,TeamLeader- LCMS /John M.Flaherty,Vice-/President OtherLabMembersContributingto Data KarenRisha Date Date t '1 " PAGE 5 OF 5 R II I ii SECTION A I EvgenTM . Proven Results. Summary of PFOA, PFHS, PFOS and FOSA in Water Samples Sample ID BC2 SW-04 BC2 SW-04* BC2 SW-04 Dup BC2 SW-05 BC2SW-05* BC2 SW_05 Dup BC2-SV-06 BC2-SW-06* BC2-SW-06 Dup Outfall to River $W-25 Outfall to River SW-25" Outfall to River SW-25 Dup Equipment Blank-Pump Equipment Blank-Dredge Field Control/Travel Blank Analyte C8 Acid PFOA PerfluorooctanolcAcid 4.21 4.21 2.54 0.591 0.616 1.56 12.1 12.3 11.6 15.8 Found (ng/mL) C6 Sulfonate PFHS Perfluorohexanesulfonate 0.896 0.882 0.571 0.155 0.152 0.377 6.06 6.30 5.87 7.66 16.0 7.10 14.4 6.77 ND ND ND ND ND ND Sample ID BC2 SW-04 BC2 SW-04* BC2 SW-04 Dup BC2 SW-05 BC2SW-05* BC2 SW-05 Dup BC2-SW-06 BC2-SW-06* BC2-SW-06 Dup Outfall to River SW-25 Ouffall to River SW-25" Ouffall to River SW-25 Dup Equipment Blank-Pump Equipment Blank-Dredge Field Control/Travel Blank Analyte Found (ng/mL) C8 Sulfonate PFOS FOSA PerfluorooctanesulfonatePerfluorooctanesulfonylamide ' 11.5 1.39 ' 11.5 1.37 8.25 ,1.67 0.790 0.146 i.54 0.150 4.33 0.389 26.1 2.43 26,7, 2.30 25.1 2.57 31.2 3.26 31.5 3.18 30.8 3.28 ND ND ND ' ND ND ND ND=Not Detected=Response between 0 and 0.025 ng/mL NQ=Not Quantifiable=Response between 0.025 ng/mL and LOQ (0.05 ng/mL) "Laboratory Duplicate I p " _305B .dr _iState I 1L.T: _F: ResearchDrive College,PA 16801, USA 814.272.1039 814.231.1580 exygcm.com I I I I STANDARD TERMS AND CONDITIONS Services provided by Exygen Research are limited to the terms and conditions stated herein, unless otherwise agreed to in a formal contract. ONFIOENTIAI.ITY--Exy#en Research ("Exygen." "us," oi ':we"} maintains the strictest confidentiality in all of our client interactions. If a signed confidentialily agreement is required, we will provide one. If a regulalory or legal body subpoenas informa.tion, the chenl will be nobfied p,omptly, The client agrees not Io use Exygen's name and;or data in any manner that migh! cause harm to Exygen's reputation or husio,ess. Apillro_,al must be obtained, in writing, before E_vgen's name c_m.be published in ai_y way CONTRACTS--A!I Contracts are subject to tewew and approval by Exygens leBa] council and must be signed by a co_porate officer. PAYMENT l'ERwiS--Un!ess otherwise set forth ic, this Purchase Order, terms of Qaymeni are "Net 30 Days." Tl,e time allowable for payment sh.lll begin after both' (a) dieut s receipt o'_E._,igen'sinvoice; and (b) the satisfactory performance of the services contemplated hereunder. A 1.5% monthly service chalge shall be added to all past due balaaces Notwithstanding any paymeot forms to the contrary set forth in this PurchaseOrde,: Exygen, in its sole discretion _eservesthe right to request payment in advance from client In tl_e event o; default in payment for services rendered, Eygen shall be entitled to reasonable costs of collection, ii_duding, but not limited to, attorneys' fees. BILLING--All fees and charges are billed directb/to the client req_esi ng servkes. L:xygenwill not bill a third party without prior notificalion in writing, vi_] a signed statement acknowledging and acceplinq _esponsibilil_, fl_r payment. Exygen will assume that the paperwork submitted with a sample describes the desired testin_ protocol. Any changes to the Dotocol must be submitted in writing Pleasefax changes t(:_Exygen marked, "URGENT" to your assigned representative. If changes are made after the or g hal y requested testing has been initia_ed or completed, the client accepts responsibilib/ for payment. Exygen will not be responsible for hold times that are missed due to such changes. RUSH EERVlCE--Exygen routinely offers expedited l:umaround times on critical analyses. Rush analysisservices are contingent upon availability and prearrangement with an authorized Exygen represenlative. A sulcharge is usually added Lo the list fee if rush analysis is requested, WIINIWIUM FEE--The minimum fee for commelcial services is one hundred dollars ($I00). SAWIPI.COLLECTIONI'SUBAdlSSIO,M--Client shall be responsible for proper col!ectioi_, preservation, packing and packaging, and shq]ment of the sample(s) in accordai_ce with applicable law and good commercial practice. Title and risk of loss with respect to submitted samples shall at all times remain with client prior to acceptance by an Exygen sample custodian. Exygen will initiate a chain-of-custody upon san]ple receipt unless the client includes one with the sample('s). By request, Exygen will provide chain-of-custody forlns ,_orclient's use, All samplessubmitted must be accompanied by: purchase o,'der, el signed auolation sample description, including sample type, source, hme and date o collection: specific anaiyses requested; estimated concentration levels; _eques.tedreport date; current biffing address; and other relevant information Upon request, Exygen will provide and ship appropriale sample containers to clients. _l_ese 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 requestin_ overnight delivery of sample containers will be invoiced for freight. Exygen reserves the right to charge a fee for sample containers, SAA4PLE DISPO.AL--Exygen retains samples for one month after reportin_ resull.s, then disposes of or returns the sample. Unless the client req.esthts._._t es_,.,pl_bi_s,e_.,r,leo_,lp, ,io_r,ra._emhe_,_vlse_ee. made for long-lelrn stoi'agc, Exy_en shal dispose of the sample(s). Exygen shall ctlarg(_a monthly tee for lone-term storage. Samples found or suspected lo eontaiu hazardous waste. ,_cco_dingto definitions _ sL_tc aa" ,'or federal guidelirles, will be rerurneu [o the client upoq coral:lotion of ff_ aoaty.qs The.cost of TetuTnin_the sample(s) will be invoiced lo ]he client. Exygen leserves the right to charge a disposal lee for the d sposa of any and all so'..,npl_'usnless returned by Exygen to client Eygen shall, unless the nature and character of the sample dictates otherw,sc, store all samples under locked, temperature..conbolled conditions. Ac inlernal chain-ofcustody is malnLa.incdfor each Io[ of samples received. HAZARD COMMUNICATION--The c!_enthas the responsibility to inform the laboratory of an,.-k' nown or suspected hazardou_ characteristics at the sample, and to provide information on hay_ardprevention and personal protection as necessary el otherwise required by applicahle law. QUALITY"ASSURANCE-.-Eygee will perfm m serv cos cot sistenf with its QL,a_i.yAssurance Sta,_.dad Oi)eratmA Procedures (SOPs'Lthe terms of whici! are exp!essly incorporated herein by rcfereilce: provided, however. _i shaNbe the exclusive responsibdily oi the client _o confirm that Exygen's standard practices will meet the chenl's needs prior to placing an older for wodc In the event client desires ar_allernative to these SOPs. such requests must be made in writing prior to, sample submisslon and acceptance by Exygen. ETHICY POZ/CY--Exygen Research strives 1o provide its cheats vvilh lhe highest quality data in the faslest reahsiic turnaround time. We balance I the high standards of this goal by insisting that each employee also ] perlorm within the guidelines el the highest possible professional elhics. Each Exygen employee is required to sign a stateme.t el pc'rsona[ and professional integrity SPECIAL REPORYS.-Addif.ionat charges may be nece%aryfor 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 _elating to work performed by Exygen Researchshall ,heinvoiced by Exygen and p,t,d 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, INDEWINIFICAT/ON, L/ABILITY. AND INSURANCE--Exygen agrees to indemnify, defend, and save the client, is office]s, directors, employees, alfents, and representatives harmless from all losses, expenses, demands. arid claims made a,_ainst the client, _tsofficers, directors, emplovees,._gents and represenLrtives because of any l._ersonalinjmies, dealh, or properly damage to the exl.ent caused by lhe neghgence o, willful nlisconduct of Exygen. its emplovees a.?,enls or representatives in connection with the performance of services under this agreement, except to ti_e extent such losses, expenses, den]ands, or claims, occur as a result of the negli}ie_t or willfLil acts or omissions of the client, its officers, directors, employees, agents, and representatives; howevec such indemnification and damages shall, in the aggregate, be limited to the amount equal to the lesser of (a) damages suite.led by the client as the direct result thereof, or (b) the tot_l amount paid to Eygen for [he work herein covered. Exyge_]will. if requested by the client, furmsh certificates of insurance from its carrier evidencing appropriate insurance coverage WARRANI'YAND L/WIITS OF LIAEILIFY-.--In aecept.ing-analytical wo_k, Exygen gualantees the accuracy of the test resulls for .Hiesample as submitted within the toietances set fort,_ in the SOPs We disclaim any o_her warranties, expressed or ,'nplied by law. Exyge_;does not accept any legal responsibili_ for Uie puiposes for which client uses the lest results. Exygen will not accep_any purchase order or any other order for work that includes conditions ]hal vary from these Standard Conditions. ACCEPTANCE OF PURCHA..CEORDER.--This PurchaseOrder becoines a _, binding agreement, subject to the specificterms and conditions stated herein, upon Exygen's commencemen_ of work. i i | I E genHMc Proven Results. I II I .. Summary of PFOA, PFHS, PFOS and FOSA In ,_I Samples Sample ID BC2 SED-04 BC2 SED-04* BC2SED-05 BC2 SED-05* BC2-SED-06 BC2-SED_06* Ouffallto River SED-25 Outfa(Ito River SED-25* Ouffall to River SED-25 Dup Analyte Found (ngJg, as received) C8 Acid PFOA C6 Sulfonate PFHS PerfluorooctanolcAcid 3.02 2.14 5.14 4.41 14.2 13.6 10.7 7.59 Perfluorohexanesulfonate 0.566 0.413 1.45 1.75 2.46 2.61 3.19 2.26 17.7 4.98 t Analyte Found (rig/g, as received) Sample ID BC2 SED-04 C8 Sulfonate PFOS Perfluorooctanesulfonate 14.6 FOSA Perfluorooctanesulfonylamlde 7.15 BC2 SED-04* " 11.9 7.84 BC2 SED-05 " 22.8 7.86 BC2 SED-05* 25.0 12.1 BC2-SED-06 880 71.4 BC2-SED-06* 992 83.2 Ouffall to River SED-25 ". 107 28.0 Ouffall to River SED-25* ...72.1 23.5 Outfall to River SED-25 Dup 140 35.7 ND=Not Detected=Response between 0 and O.2 ng/g NQ=Not Quantifiable=Response between 0.2 ng/g and LOQ (0.4 ng]g) Laboratory Duplicate _3058 ResearchDrive _tate College,PA 16801, USA 1L,T: 814.272.1039 I&,F: 814.231.1.580 ex3_n.com I i STANDARD TERMS AND CONDITIONS Services provided by I:xygen Research are limited to the terms and conditions stated herein, unless otherwise agreed to in a formal contract. CONF/DENTIALITY--Exygen Research ("Exygen,' "us," or "we") maintains the strictest com:iclentialiWin all of oul client interactions. If a signed confidentiality agreement _s_eq_irt,d. wn will provide one. If a regulatory or legal body subpoenas information, the client will be notified promlatly. The client agrees not to use Exy_,en'sname and,,'or data in any manner that might cause ham1 to Exygen's reputation or business. Approval must be obt?,ined, hr writing., before Exygen's name can be published in any way CONTRACTS--All contracts are subject in :eview and apDoval by Exy_en's legal council and must be signed by a corporate officer. PAYMENT TERA4S---UnIessotherwise set forth in this Purchase Ordeh terms of pnymenl are "Net 30 Days " 1he time a.llowable fo_ payment shall begin alter both: Ca1clie.nl's receipt of Exy_en's invo!ce; 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 lerms to the contrarv set forth in this PurchaseOrder, Exygen. in its sole discretion, reserves the right to request payment in advance from client In the event ot detault _npayment for services rendered. Exygen shall be entJlled to reasonable costs of collection. including, but not limited to, attorneys' fees. BILLING---All fees and charges ate billed direclly Io the client requesting services. Exygen will nol bill a third pad.y wifl_out prior notification _n writing, via a signed stalement acknowledging and accepting _esponsibility for payment. Exygen will assume that _l]e paperworl.<submi_ed with a sample describes the desired te._ting protocol. Any changes to the protocol must be submitted in writing. Please fax changes to Exygen marked, "URGENT" to your assigned representahve. If changes are made after the originally requested testing has been inihated or completed, the client accepts responsibili_ for payment. Exygen w_ll 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 aut.horized Exygen representative. A surcharge is usually added to the list lee if rush analysis is requested, MINIMUM FEE--The minimum fee for commercial services is one hundred dollars ($100). SAMPLE COLLEC'-TION/SUBMISSION--Client shall be responsible for proper collection, preservation, pacldng and packa,Ring,a_cl shipment of the sample(s) in accordance with applicable law and good commercial practice. Title and risk of loss with respect to subnfitted samples shall at all times remain with client prior _.oacceptance by an Exygen sample custodian. Exygen will initiate a chain-of-custody upon sample _eceipt unless the client includes one with the sample(s). By request, Exygen will provide chain-of-custody lorms for client's use AI! 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 billitlg address: and other relevant information Upon request, Exygen will provide and ship appropriate sample containers to clients. These containers will include the appropriate preservative if particular analyses require one. It is the responsibility of the client to handle these preserved containers safely, and using all appropriate safety precautions. Clients requesting overnight delivery at sample containers will be invoiced for freight. Exygen reserves the right to charge a fee for sample containers, SAMPLE DISPOSAL--Exygen retains samples for one month after reporting results, then disposes ot or returns the sample. Unless the client requestthsatthesamplebcs_lr.eturneodr, pdorarrongemeh,,atsve_een made for long-term stara_'e. Exy_on shall dispose of tJ_esarnp!e(s). Exygen shall charge a rnonlhly tee iol Iong-t_:'rm storagr,. Sampk's foLmd rJr suspected to co_t:._n hazardous w%te. a.cc)td_u_to d_(initions ir_sh",tc ar ,,'or (ederal guidelines, will be. returned to the client upon completion o_ tt_ analys_s.The co_t of returning the _ample(s) w_ll be invoiced In the client Exygen reserves the right to ch,'age a disposal fee fol the dispgsa_of any and all sampies unless rewmed by Exygen In cl_ent. Exygen sl_all, unless the r_.atuteand character el the sample dictales otherwise, store all samples under locked, temperature-controlled conditions. An internal chain-of- cus[l:_dyis maintained for c'ach lot at sampl_:sreceived. HAZARD COMMUNICATION--The client has the responsibility to, inform the laboratory.'ot any known or s'qspectedhazarckxJscharacterislics _f the sample, and to provide inlormation on hazard prevention and personz_} ptotectiotl as ne.,:essarvol otherwise required by applicable,law QUALITY ASSURANCE---Exygen wdl _}erfom services co_sistent with t_ Quality Assurance Standard Operahng Procedures (SOPs).the temps ol which are expressly incorporated herein by re_erence: provided hpweveh it shall be the eclusive responsibility of the client to cor_f_rmthat Exyge_'s sta_dard practices will meet the client's needs Dior to placing _.',norder for work. In the event client desires an alternative tn these SOPs. such requests must be made in writi_g prior to _ample submissio_ aud _cceFt,ance by Exygen THIC.CPOLICY--Exygen Research strives to provide its clients with the highest quality data in the fastest reahstic turnaround time. We balance I the high standards of this goal by Jnsisthlgthat each employee also perlorm within the guidelines of the h_ghestpossible professional ethics. Each Exygen employee is required to sign a statemenl of personal and professional in_t_gfit'y. SPECIAL R_PORT.,C--Additiooal charges may be necessary for custom _eport formats. LITIdATION--All costs associ,_,tedwith compliance Io any subpoena to_ " NI documents, for testimony in a court of law, or for any other purpose re ating to work performed by Exygen Researchshall 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 accommodalions, and for any and all other expenses associated with said litigation. INDEMNIFICATION, LIABILITY, AND INSURANCEJ-Exygen agrees to indemnify, defend, and save ti_ client, ils off_ce1s,d_rectors, employees, agents, and representatives harmless from all losses, expenses, demands, and claims made against the client, _lsofficers, directors, ernployees,.agents and representatives because of any persona_ iniunes, death, or property damage to the extent caused by ffw negligence or willlul misconduct oi" Exygen, its employees, a_ents, or _epresenta_ivesin connection with the performance of services unde_ _his agreement, except to the e_ten[ such losses, expenses, demands, or claims, occur as a result of the negligent o_ willful acts or omissions of the client, its officers, directors, employees, agents, and representatives: however, such indernnihcation and damages shall, in the aggregate, he limited to the amount equal to the fosse,of Ca) damages suffered by the client as the clirect result thereof or Lb)the total amount paid to Exygen for the work hereto covered. Exygen will if requested by the client, furnish certificates of insurance from its ca_fier evidencing appropriate insurance coverage. WARRANTY AND LIMITS OF LIABILITY_In accepti_l_ arlalylical wot k, Exygen guarantees the accuracy of the test :esults fo_ the sample as submitted within the tolerances sei fe,rth in the SOPs We disclaim any other warranties, expressed or implied by law. Exygen does not ,_cceptany legal responsibility for the purposes for which client uses the Lestresults. Exygen wilt not accept any purchase order or any other order for work that includes conditions that vary from these Standard Conditions. ACCEPTANCE OF PURCHASE ORDER--This Purchase Order becomes a._ binding agreement, subject to the specific terms and conditions stated herein, upon Exygen's commencement o| work. E I II I en ProvenResults. I |1 Summary of PFOA, PFHS,PFOSand FOSA in_1_ Samples Sample ID BC2 SED-04 BC2 SED-04* BC2 SED-05 BC2 SED-05* BC2-SED-06 BC2-SED_06* Ouffaltlo RiverSED-25 Outfaltlo RiverSED-25* Ouffallto RiverSED-25 Dup Analyte Found (ng/g, dry weight) C8 Acid PFOA PerfluorooctanoAlcid C6 Sulfonate PFHS Perfluorohexanesulfonate 4.31 3.06 0.809 0.591 7,39 2,09 6.34 2.51 23.6 4.08 22.5 4.33 16.9 5.05 12.0 3.57 26,2 7,39 _mq Sample ID BC2 SED-04 BC2 SED-04* BC2 SED-05 BC2 SED-05* BC2-SED-06 BC2-SED-06* Out/allto River SED-25 Out/allto River SED25* Out/allto River SED-25Dup Analyte Found (ng/g, dry weight) C8 Sulfonate PFOS FOSA Perfluorooctanesulfonate 20.9 17.0 i 32.8 36.0 1460 Perfluorooctanesulfonylamide 10.2 11.2 11.3 17.4 118 1640 138 ' 169 44.3 114 37.2 208 52.9 ND=NotDetected=Responsbeetween0 and 0.2 ng/g NQ=NotQuantifiable=Responsbeetween0.2 ng/gandLOQ(0.4 ng/g) *LaboratoryDuplicate " _3058 ResearcDhrive _' '_hiStateCollegeP, A16801,USA 1L.T: 814.272.1039 _F: 814.231.1580 exygen.com I II I II STANDARD TERMS AND CONDITIONS Services provided by Exygen Research are limited to the terms and conditions stated herein, unless otherwise agreed to in a formal contract. CONFIDEN1"IALIT_---Eygen Research("Ex_gen," "us," or "we") maintains the strictest confidentiality m all of ou_ client interactions. It a signed confidentiality a_;reemenr Is required, we will provide one. if a regulatory o_ legal body subpoenas inlormafion, tl_e client will be notified promptly, The client agrees not to use Exyg,en'sname afld,."ordata in any Inanner thai might cause harm to Exygens reputation o_ husine%. Approve! must be obta,led, in writing, before Exygen's name can be published in any way CONTRACTS----Allcontracts are subject to review and approval by Exygen's legal council and must be signed by a corporate officer. PAYMENT TERMS---Unless otherwise set forU: in this P_rchaseOlder, terms of: payment are "Net :30 Days ' The time allowable for payment shall begin niter both: (,_)ciient's receipt of Exygen's invoice; and (b) tl_e satisfactory performance of the serwces contemplated hereunder. A 1 5% monthly service charge shall be added to all past due balances, Notwithstanding any payment lerms to tl_e contrary set forth in tNs PurchaseOrder. Exygen, in its sole discretion, reserves the right to request payment in advance from client, in the event of ddault in payment for services rendered. Exygen shall he entitled to reasonable costs of collection, including, but not limited 1o. attorneys' fees, BILLINC_--AII tees and charges are billed directly to the client requesting services. Exygen w_ll not bill a _ird p_rty without prior notitica_.ionin writin_ 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 ta the protocol must be submitted m writing. Pleasefax cl]anges to Exygen marked, "URGENT" to yau_ assigned representative, If changes are made after the originally requested testing has been iniha[ed or completed, the client accepts responsibility for paw_ent. Exygen will not be responsible lot 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 purseuaarlrlyanagdedne_detnot wthiteh liasnt laeuethiforriuzsehdanEaxlyygseisnisrerepqreuseesntetadt,ive. A surcharge is MINIMUM FEE-The minimum fee for commercial services is one hundred dollars ($100). SAMPLE COLLECtION/SUBMISSION--Client shall be responsible for proper collection, preservation, packing and packaging, and shipment of the sample(s) in accordance with applicable law and good commercial prac'[ice. Title and risk of losswith respect to submitted samples shall al all times remain with client prior to acceptance by an Exygen sample custodian. Exygen will initiate a chain-of-custody upon sample receipt unless the client includes one witl_ the sample(s). By request. Exygen will provide chain-of-custody forms for client's use. All samples submitted must be accompanied by: purchase orcJe_o;r signed quotation: sample description, including sample type, source, time and date of collection; specific analyses requested, eslimated concentration levels; requested report date; current billing address; ,lad other relev,mt information, Upon request. Exygen will provide and ship appropriate sample containers to clients. These containers will include the appropriate preserval_ve if particular analyses require one. It is the responsibility of tile cheat to handle these preserved containers safely, and using all appropriate safety precautions. Clients requesting overnight delivery of sample containers will be invoiced for frei_ht. Exygen reserves the right to charge a fee _orsample containers, SAMPLE DISPOSAL--Exygen retains samples for one month after reporting resuks, then disposes of or returns the sample. Unless the client req.es:htsatthe_.,mpleb_erselturneodrp,co,ra,r_,l_.enh,_e,..bteseen made for long-term storage. Exygen shall dasposeel the sample(s) Exygen shall charge a monlhly fee k)t lone-term storage. Snmptesrotund or suspected to contain haza_duus waste, according to defin,tions in state at" .,'or federal guidelines, wiil be returned to _:heclJ.t'ntupon completion of t,_l am]lysls. The cost of returnino the sample(s) will be invoiced to the client. Exygen reserves the .ght to charge a disposal lee [nr the disposal of any and all samples unless returned by Exygen to client, Exygen shall, unless the nature _..ndcharacter of the sample dictates otherwise, store all samples under ocked, temperature-onto led condihon_ An in_cr,nal (:hair,-of- custody is maintained for e_{chlot of samples _,ceived. HAZARD COMMUNICATION--The client has the tespons bilty to inform the iabor,_tor_/of any known c,r suspected hazardous characteristics of the sample, _u_d[o provide' information on hazard prevcnhon ,,nd personal protection as necessary o_ otherwise required by e,ppii_abie law. QUALIPr" ASSURANCE--Eygc.n will perform services consistent with its Quality Ass_rance St,',ndard Operatin_ P_ocedures('SOPs),the terms el which are epfessly incorporated herein by' reference; prowded howeveh ;t _ha!l be tlle exclusive responsibility of the ellen! kocot',firm tl_at Exygen's standard pt,lctic.es will meet the clienl's needs iMor to placing an order for work In the event client desir(,s ,m alle_nalive to tl_eseSOPs, such requests must be made in writing prior Io sample submission and acceptance by Exygen. ETHICS POLICY--Exygen Researchstrives to p_ov_deits dierfls with the highest quality data in the fastest rr:alislic turnaround time We balance I the high standards of thk gcai by insisting Iha_ each emplo_/eealso ] perform within t'he guidelines of the hi_ilest possible profession,:l ethics, Eitch Exygen employee is required to sign a statement of personal and professional integrity. .qPECIALREPORT.C--Additional charges may be necessaw for custom report formats LITIGATION--All cosls associated with compli,_nce Io any subpoena for _I documents, for testimony in a court of law. or for an,_other purpose ;elating to work performed by Exy_en Research shall be invoiced by Exygen and prod by client. These costs shall include, but me not limited to. hourly charges for the persons inv(flved, travel, mileage, and accommodations, and fo_ an), and all olher expenses associated with said libgation. INDEMNIFICATION, LIABILITY. AND INSURANCE--Exv,_"en 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, d recto s employees,,_gents and representatives because of any personal in,jurms,death, or properb/ damage [o the exl.ent caused by the neghgence or willful miscondud of Exygen. its employees, agent_, or representatives M c<_nnectionwith the performance of services under this agreement, excep_to the extent such losses, expenses, dem4nds, or claims, occur as a result of the negligent or willful acts or omissions o! tile client, its officers, directors, employees, agents, and representatives; however, such indemnification and databases shall, in the aggregate, be !imited to the amount equa_to the lesserof (a) damages suffered by"the client as the direct result thereof, or (L,)the total amount paid to Exy@enfor the work herein covered, Exygen will, fl requested by the client, furmsh certificates of insurance from its carrier evidencing appropriate insurance coverage. WARRANTY*AND LIMITS Of LIABILITY--In accepting analytical wo, k. kxygen guarantees the accuracy of the test results for the _ample as submitted within the tolerances set forth in the SOFs.We disclaim any other warranties, expressed or implied by law Exygen does not accept any legal responsibility for the purposes for which c!ient uses the test results. Exy_en will not accept any purchase order or any other order for work that includes conditions that w_ry from these Stand,_rdConditions. ACCEPTANCE OF PURCHAEE ORDER--This PurchaseOrder becomes a binding agreement, subject to tt]e specific terms and conditions stated "_ herein, upon Exygen's commencement of work. El I__ l I l II Illl II II I SECTION B i I W l_ Precise Research - Proven Results. RecoverySummaryforPFOA,PFHS,PFOS8ndFOSAInWater I '. _.. Sample ' Description BC2 SW-04 Lab SDike BC2'SW-04 Low Spike BC2 5W-O4 High Spike Amount Spiked (ng/mL] C8 Acid PFOA Amt Found Amount In Sample Recovered (nq/mL) (ng/mL) 5 4.21 8.14 Recovery (%) Amount Spiked (ng/mL) C8 SuIfonats PFHS Amt Found Amount In Sampie Recovered (ng/mL) (ng/mL) 79 5 0.696 5.52 Recovery (%1 92 0.1 4.21 10 4.21 2.76 -1450" 0.1 9.92 57 10 0,898 0,896 0.647 9.73 -249* 88 BC2 5W-05 Lab Spike BC2 SW-G5 Low Sp_ 5 0.591 0.1 0,591 4.96 87 5 0.155 5.00 97 2,17 1579" 0.1 @155 0,607 452 BC2 SW-05 High Sp_u BC2 SW-06 LabSpike, 10 0.591 5 12,1 7.21 66 10 O. 155 17,8 114 5 6.06 9.58 94 11.8 115 BC2 SW-06 Low S_ke ' 0.1 12,1 BC2 SW-06 High Sp4ke ". 10 12.1 13.9 1800" 0.1 6.06 24.2 121 10 6.06 7.11 1050" 17.4 113 Oullell Is RiverSW-25 Lab Sp_xe !. 5 15.8 C_dslt to Riv_ SW-25 tow Spike O.1 15.8 Oudail to RiverSW-2$ High Spil_ 10-. 15.8 22.1 126 6 7.66 15.0 -800" 0.1 7,66 26.2 104 10 7,66 12.2 91 6.64 -1020" 18,1 104 FieldConUol/Trave};tlsnk Low Spi_e 0.1 ND 0.114 114 0.1 NO 0.119 119 Fl_ld Contro_TravelBlankHigh Spike 10 ' ND 11.9 119 10 NO 10.8 108 C8 Sulfonate Pros FOSA Sample Description BC2 $W-O4Lab ,Sp_ke BC2 SW-04 Low Spike BC2 SW-04 HighSpike BC2 SW-05 lab,Spike BC2 SW-05 Low Spike B.C2 $W-05 High Spike BC2 SW-06 LabSpike BC2 SW-06 Low Spike Spiked Amount , (ng/mL) in Sample Recovered And Found Amount (ng/mL) .. (rig/roLl Spiked Recovery Amount (%) : (n_mL} In Sample Amt Found (ngfmLI Recovered Amount _ng/mL} Recovery _%1 5 11.5 '. 17,1 112 5 1,39 5.58 84 0.1 11.5 10 11,6 6.89 "4610 0.1 1.39 17_7 62 10 1.39 0.672 7.18 o718" 58 5 1.67 5.94 ' 85 5 0.146 4.86 94 0.1 1.87 10 1.67 5.37 " 3700" 0,1 12.8 111 10 0.146 0.146 0.498 352 4.14 40 25 26.1 0.1 26.1 49.8 95'. 5 2.43 32.1 6000" 0.1 2.43 7.18 95 2.55 120" BC2 SW-06 High Spike 10 26.1 Otaf_ to RJ,_r SW-_ tab Spike 50 31.2 Outf_JIto River SW.25 Low Sp_ke 0.1 31.2 43.9 178 '.. 10 2.43 80.9 99 5 3.26 29.4 -1800" 0.1 ' 3.25 8.44 60 7.97 94 2.66 -600" Outfaa_oRiver 5W-25 High Splka 10 31.2 Fie_l ControiitTravelSI_k LowSpike 0,1 NO F'NlldCoI_uo_/Tarvel BIg/ikHigh Spike IO NO 41.2 0.109 11.4 100 10 . 3.26 9.02 58 109 O.1 "-.ND 0.0898 90 114 10 NO 11.9 119 NO,,Not Detecte<_sRespollaabetween 0 _ 0.025 no/mL N_Not (_JanUfla_=Respor_a betW_iln0.re5 ng/mLarid LOCI(0.05 nOh'_.). ",. ".. "Sample residue sign_canlfy exceeds the spiking level; therefore, an accurate recovery cannot be ca_.u|ated. ,_1_k_V05_ ResearchDrive _h_tate College,PA16801, USA 814.272.1019 exygen.com II I I j Precise Research Proven Results. Recovery Summary for PFOA, PFHS, PFOS and FOSA in Soil . ' Sample ". De,,scr, iption . BC2SED-04LabSpike. Amount Spiked (ng/g) C8 Acid PFOA Amt Found Amount 'Amount in Sample Recovered Recovery Spiked (ng/g) (ng/g) -. .... (%) (n_/g) C6 Sulfonate PFHS Amt Found Amount in Sample Recovered Recovery (nglg) (nglg) (%) 40 3.02 41.5 96 40 0.566 42.2 104 BC2SED-05LabSpike 40 5.13 43.7 96 40 1.46 44.2 107 BC2SED-06LabSpike " 40 14.2 49.4 88 40 2.46 44.5 105 Ouffaltl o RiverSED-25LabSpike 40 10.7 47.1 91 40 3.19 44.5 103 Sample Description . C8 SulfonatePFOS Amount Amt Found "Amount FOSA Amoul_t Amt Found Amount Spiked in Sample Recovered Recovery Spiked in Sample Recovered Recovery (ng/g) .. (ng/g) (n_/g) (%) (nglg) (ng/g) (ng/g) (%) BC2SED-04LabSpike 40 ' 14.6 51.8 93 40 7.15 46.5 98 V 8C2 SED-05LabSpike 40 22.8 61.0 95 40 7.86 48.1 101 BC2SW-06LabSpike 800 88_) 1720 105 800 71.4 650 72 Outfaltlo RiverSW-25LabSpike 40 107 . 153 114 40 28.0 59.0 77 =r Resultsreportedonanas-receivedbasis V .. 058 ResearchDrive te College, PA 16801, USA : 800.281.3219 F: 814.272.1019 exygen.com SECTION C I_ I I II Ill ii iii i i i ii iIli I I II 7/21/2003 lof3 3M ENVIRONMENTAL LABORATORY "_ Prelimhmry/Unauthortzed Report Project: E03-0561 Requester. Schnobrich, Dana M (223-1N-08) Department: 530711 Project Number:. 0022674449 Date Received: 6/26/2003 Project Dcscription: Decatur Bakers Creek #2 Surface Water and Sediment Comments: Proleet Results/_tiviry Pace Field Sampling Event Completion Date: Project Lead: Jess S. Eldridge Phone Number:. 651-778-5233 Email Address: jscldridgc@mmm.com _qag _ob3"_ e'_ y._,',_ lgll W_4kCr _< 1'*_' p_r,t', )"_ -f_ poTtt/" .... C_(_Jo-) 3M Sample Number E03-0561-49786 Sampled Date 7/22/2003 Sample Description BC2 SW-04 LAB EXYGEN EXYGEN Analytical Mcth0_ PFOS by ESMS PFHS Comeonents PFOS PFHS Result RL EXYGEN FOSA FOSA ] EXYGEN PFOA PFOA 1 E03-0561-49787 7/22/2003 BC2 SW-04 DUP LAB EXYGEN Analytical Method PFOS by ESMS _t_ EXYGEN F..XYGEN EXYGEN PFHS FOSA PFOA E03-0561-49788 7/22/2003 ._,.gJI_ZQfI,gI H PFOS PFHS FOSA PFOA BC2 SED-04 Result RL LAB EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS EXYGEN FOSA EXYGEN PFOA EO3-O561-49789 7/22/2003 Comnonents PFOS PFHS FOSA PFOA BC2 SW-O5 Result RL LAB EXYGEN EXYGEN EXYGEN EXYGEN E03-0561-49790 Analytical Method PFOS by ESMS PFHS FOSA PFOA 7/22/2003 Comeonents PFOS PFHS FOSA PFOA BC2 SW-05 DUP Result RL Ouallfler LAB EXYGEN EXYGEN EKYGEN EXYGEN E03-0561-49791 Analytical M_t_od PFOS by ESMS PFHS FOSA PFOA 7/22/2003 (_omnonents PFOS PFHS FOSA PFOA Be2 SED-O5 Result RL LAB EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA 9mnonents PFOS PFHS FOSA RHult RL 7/21/2003 !_;*" 3M ENVIRONMENrAL LABORATORY Preliminary/Unauthorized Report Project: E03-0_l (cont.) 3M Sample Number E03-0561-49791 (cont.) Sampled Date 7/22/2003 Sample Description BC2 SED-05 LAB EXYGEN Annlvtlq;nlMethod PFOA E03-0561-49792 7/22/2003 Comnoneots PFOA BC2 SW-06 Result 2 of3 RL Oaalifler LAB EXYGEN EXYGEN EXYGEN EXYGEN Analytical Mttho4 PFOS by ESMS PFHS FOSA PFOA E03-0561-49793 7/22/2003 Components PFOS PFHS FOSA PFOA BC2 SW-06 DUP Result RL LAB EXYGEN EXYGEN Analytical Mefhod PFOS by ESMS PFHS Components PFOS PFHS Result RL EXYGEN FOSA FOSA _ EXYGEN PFOA PFOA t E03-0561-49794 7/22/2003 BC2 SED-06 LAB EXYGEN EXYGEN EXYGEN Analytical M_hod PFOS by ESMS PFHS FOSA EXYGEN PFOA E03-0561-49795 7/22/2003 LAB EXYGEN EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA PFOA E03-0561-49796 7/22/2003 LAB EXYGEN EXYGEN EXYGEN Annl,/ticol Method PFOS by ESMS PFHS FOSA EXYGEN PFOA E03-0561-49797 7/22/2003 LAB EXYGEN Analytical Meth0_ PFOS by ESMS EXYGEN EXYGEN PFHS FOSA EXYGEN PFOA E03-O561-49813 7/22/2003 LAB EX'YGEN Analytical MEethpd PFOS by ESM$ _1_ EXYGEN EXYGEN EXYGEN PFHS FOSA PFOA Comnonenu PFOS PFHS FOSA PFOA OntfaH to River SW-25 Comnonents PFOS PFHS FOSA PFOA Ouffall to River SW-25 DUP Components PFOS PFHS FOSA PFOA Ontfali To River SED-2$ Comoonents PFOS PFH$ FOSA PFOA Outfall to River SED-25 DUP Comoonents PFOS PFHS FOSA PFOA Result Result Result Result R_alt RL Oualifler RL RL RL Oualifler RL 7/2]/2003 3M ENVIRONMENTAL LABORATORY Prelbnl.mT/UuutborlzReedport Pro|ectE:03-0_I (_.t) 3M Sample Number E03-0561-59479 Sampled Date Sample Deteription Field Control/Travel Blank LAB EXYGEN EXYGEN EXYGEN EXYGEN Annlvtieal Method PFOS by ESMS PFHS FOSA PFOA Components PFOS PFHS FOSA PFOA E03-0561-59480 Equipment Blank - Pump LAB EXYGEN EXYGEN EXYGEN EXYGEN AnnlvttcaI Mfthod PFOS by ESMS PFHS I_OSA PFOA E03-0561-59481 EXYGEN EXYGEN EXYGEN EXYGEN Analytical, Method PFOS by ESMS PFHS FOSA PFOA Compon_nt_ PFOS PFHS FOSA PFOA Equipment Blank - Dredge ComnonentJ PFOS PFHS FOSA PFOA Result Result Result 3 of 3 RL RL Oeallfler RL V 3058 Research Drive Phone: 800-281-3219 Eygen State College, PA 16B01 Fax: 814-272-1019 _j/' RESEARCH ' _. i Laboratory Sample Lo_l-in Sheet (Environmental_ Complete upon .sample receipt: Client and/or . i Method of Oellvery r3 Walk-in Tracking #:. O Pick-up 7/-/r/_"/_/P DUPS 8' F. _./2_ --,2_EX. #(: [] Air Borne [] (_hsr (explain) Chain of Custody : Temperature PresePtatlon Custody Seals: C] pres_ .l_-_Tsent intact/ [] broken (explain) Thermometer ID: _'c 2. ,_7' Cooler lO: Cooler ID: Cooler ID: Cooler ID: <;" it" _._,o Cooler temp: _ Cooler ternp: --. Cooler ternp: __ Cooler temp: __ Chain o! Custody Record: .._'_resent I [] absent Samples Received: 'C "C r C C l_r"on ice in ice melt [] with ice pack [] none ECxopmlapnleatteiodnby Signature: / "" . _ate (Time")': _'2/'/? /<)_ i f / lete d.n!_$amplelog4n: ". _;L ' r" :':".:.'._;,-_-.:.' .:._,:_ . -. .'.. tJMSLog-in# Physical Condition Samples intact? I J_ [] NO {explain) / Chain of :Custody !Analysis Request ..... Preservation Samples received agree with COC record? Al_alyslrsequesctlear?. Sample containers appropriate? Chemical preservation appropdate? Samples received within holding time? Sample volume/mass adequate?. 3_es .,, _Yes [] No (explain) n No(explain) [] Yes 0 Yes 12IYes [] Yes [] No (explain) [] No (explain) 0 No (explain) [] No (explain) Completed by Signature: i = Jl Complete following resolution of any nonconformances: I Client Contacted I-I Yes [] No Client: Resolution Completed by Signature: _ - ..... Lab Sx Log-in Sheet -Ex =i Oats: /Z J/f" = i e Date (Time): 11-5-0110 .[ II I l i .i i LOGIN CHAIN OF CUSTODY REPORT (In01) Jul 28 2003, 07:54 am Account: Login Number: L34910 2046 3M ENVIRONMENTAL LABORATORY iL34.910 -1 _ >:<.i::.i....:: _ ....:BI_2 SNI-.O_.:_:::i: " ._:::i:.!i:::_:ii:i_:i!ii:ii_ii_ii%ii:_22il_5'_i_:i:__igi_3i_!_..?. < ::.::i:_ "< i: .iii.::iii_i_iiii: SAMPLES KEPT IN D0000539. L31:9_10 --:4 :._ . ,.iiB._. S_!I%_4111.?DU_IiP_ii_!_i!_/_._._U_i_!Z5_i_i_i_3i_}_ii_.}i._.i.i.i:i_.}i__:!:i:_i.ii:!...ii_i!._: SOIL S PERC SOLID Hold:01-AUG-03 d0000539 1 L:3_4910- 8 - :!:: .- B!C.:..Z. SW:.r&_O!r:5H.I,G.H S.P,K..<.- (i0.:........:.!..:_i_BIi}_-iJ<U:L2:_O{._I ?:.,_HZ..S..::.i_.J._..-...:(;:]i3:,:.":,..:.. L8 4 910 -9: -.: ." BC2 SW_O5 ..[IUP .::...:.:.:..:..i.2:!A_/_.:(]:59:1_:%%:1::_2]_{03:.:i.}:"!.!i.::.::_.:!i:-:it:>:.:.i.::..}:::::: L3 4 9.10- 10 SOIL BC2 SED:_:O5 . -. -2i-_:_:0:3:.!25-:_::O:3i./i;_:::::<.i:..<:i. i :.. S PERC SOLID Hold:01-AUG-03 d0000539 :L3..4910 -11 SOIL .{ :.. . B_2 SED:: DI6::.. :...:..: :.. .:.23::i-:_:#:_0.3.::.:2 5 -!_L ::.O:3ii:/:. S PERC SOLID Hold:01-AUG-03 d0000539 ..L .... ' ..._.>_ L,_4910.4.112 _i"-,-,..,i:_-i.,<::i....BIC2., S_i:O:6i_7: .:,: Ji_::ii!.:::._::_ii!_i_!_i-i::i:::iZ_i{_:J__:_i:!iO:.3_!{!ii_i:i:2i_5:i]_:ii_:':.":ii::::i<f::<<:::i:_i<:il/:i::_< L_3_.49TO-:I:3..I .._.BC.2S_I_:.Q::i_I:S:_.KI_:iL_OiW:_i_(_D_._::_.{_!_._i_i_i_B_i_i2i_:J:U-L__.:.:i!.:g:i_k::_:3.i_.<__i._.2 L3.4 910 - 14: " :_.. " L34910-15 .BC2 SWI-06:}<IH!.GH:III:S.pKi:i}J:u}b:}__!_{._0O:::l:-:3::!:_:i:]i__:P<B!1i)2i1_::. :2!S{!_::::.0:3 :.-<_::.:.:.IIi::!::;:L: B._2 S_[_i!0i6::.DUP::i!::::I:II_;:_<":_23:ZJU_I_03:::.25__.::.:_:7::O3.%.:"</.i.../: L34 9 I0 <! 6 .: . ..:.. O_FADL:. :_.Q:.:..:.R.IVER_::..$W_.z.2:5::_2._.i::__2:_:L3-_.-:::0.:_3..3._.:..........:....:..._ L:349{ 0-.1:7" _ - :: ....OUTF_ i_!_O_ilR_[_VE_!i:::::_-i_:._i:!0::3_21i5Zi_:J_-_i(}-3/:<[.:..:....:::, COMPLETE ID READS OUTFALL TO RIVER SW-25 LOW SPK (0.i PPB) . COMPLETE ID READS OUTFALL L3:49.10-.19: :: < TO RIVER SW-25 HIGH SPK (I0 PPB) . < _::<"i _m_ Page 1 LOGIN Account: CHAIN OF CUSTODY REPORT (in01) Jul 28 2003, 07:54 am Login Number: L34910 2046 3M ENVIRONMENTAL LABORATORY SOIL SOIL S PERC SOLID S PERC SOLID .... H01d:0i-AUGL03 Hold:01-AUG-03 d0000539 ................................. d0000539 _34-9:10-23 COMPLETE .: ..: ... :. FIiELD...::EONT_OL/T_ELI:I:BL_K:i: ._0_:::..:_23_i_[Oi_!:_i::25:.-JU_ _:O3_ ::i":,:: ID READS FIELD CONTROL/TRAVEL BLANK LOW SPIKE (0]i PPB). ........... L34:910 T24 F.I!ELD _..CONTROL/T_VEL :::B_K .:2i3-_.I_L-103: ...:.:25._4::_ 3. " ii-i.. :..:i COMPLETE ID READS FIELD CONTROL/TRAVEL BLANK HIGH S[51KE (I0 PPB). i I_3-4 910 - 25 ..:, EQUI PMENT. B_K_t_P_ I:2:1 ,:_U_:_.03...25-._L!_-O3(II:I_ . . /i. <_:.. I ii| i ........... I SECTION D r, uen P=._ .,,.. RESEARCH II I 3Rose.,eaPrhcohonnev;8e State College,PA16801 Fax: 814-231-1580 Date: 08/26/03 Exygen Study # L34910 NOTE TO FILE NOTE: i Throughout the raw data generated for study L34910 the 498 > 78 monitored transition ,_ (perfluorooctanesulfonylamide) was assigned the acronym PFOSA instead of FOSA. Any reference to PFOSA in the raw data is equivalent to FOSA. initials: ..._ 0_)/2JoI 0_ ql_l_; V Spoa._ Sh,dy NO: Exygt_ Study No: Aaalyte: lo_sMoak_i: Sire: NA [34910 PFOA 413-> 369 DecaturBak_l Creek RAW DATA REPORT Limit of Quanfitalioa: InjecfioaVolume,: Matrix: SampleV oium_.. FinalVolume:. 50 ppt 15 _ Water 40.0mL 5.0 mr_ Sot No: Analyst: Im_ Type: Exlr'_un Dale: A_Iyz_I un: 073103A KasemRisha LCdMS/MSUait # 6 07/31/03 08701-02703 Exygee f13 XC072503-0 XC072503-1 XC072503-2 XC072503-3 XC072503-4 XC072503-5 XC072503-6 MethanolWash 0106020Cun_ol 0106020 Spk A 0106020 Spk B L34910-I Spk C L34910-6 Spk D L.34910-12Spk E L34910-16 Spk F XC077..503-1 I34910-1 L34910-1 Pep L349|0-4 i.34910-2 1,34910-3 XC072503o2 ....." Spot= ID BC2 SW-04 BC2 SW-05 BC2 SW--{_ Outfal/to River SW-25 BC2 SW-04 BC2 SW-04 BC2 SW.04 Dup BC2 SW-04 Low Spk BC2 SW-04 High Spk Sample Cede CS CS C3 CS C._ CS CS C C LCS LCS LF LF LF "IF C5 S S S FP FF C__ R_m No. 073103A-100l 073103A- 1002 073103A-1003 073$03A.I004 073103A-1005 073103A-1006 073103A- 1007 073103A-1008 073103A-$009 073103A.1010 073103A-1011 073103A-I012 073I03A- 1013 0T3_'OA3 -1014 073103A-1015 073103A-1016 073103A-1017 073103A-1018 (}T5|03A-1019 073I03A-1020 073103A-I021 073103A- 1022 1.349t0-6 L34910-6 Rep L34910-9 L34910-7 [,34910-8 XC072503-3 I..34910-12 1.349i0-12 pep L34910-15 I..34910-13 L34910-I4 XCOT1503-4 I..34910-t6 ].34910-16 Rep L34910-19 L34910-17 L349tO-l_. XC077..503-5 I..349i0-25 I..34910-26 L34910-22 I "t4910-23 1..34910-24 XC071003-6 BC2 SW-05 BCT.SW-05 BC2 SW-05 Dup BC2 5W-05 Low Spk BC25W-05 High Spk BC2 SW.-06 BC2 SW-06 BC2 SW-06 Dup BC2 SW-06 Low Spk BC2 SW-06 HighSpk Ougfailto River SW-25 Ou_Jl to Rive_SW-25 Ouffa//to KiverSW-25 Dup Outt_l to River SW-25 Low Spk Outfattto P.3vcSrW-25 HighSpk EquipmentBlank-Pump Equipmc_tBinak-Dredge Ftcld Cuntrol/Ttavl Blank FwJdC.mmobTravclBhmk Low Spk lrscldConu'ol/TravetBlank High Spk S 073103A-I023 S 073103A-107.4 S 073103A-1025 FF 073103A-1026 FF 073103A-1027 CS 073103A-102g S 073103A-1029 5 073 I03A-1030 $ 073103A-1031 l_ 073103A-1032 FF 073103A-1033 CS 073103A-1034 S 073103A- 1035 S 073103A-1036 S 073103A-1037 FP 073103A-1038 _ 073103A-i039 C__ 073103A-1040 S 073103A-IO41 S 073103A-J042 S 073103A-104.3 FF 073 L03A-1044 1_ 073103A-1045 CS 073103A-1046 An_dytcFomui (pp)=,(peak area -interccpt) I slopc x DF Recovery(%) = (mud},tefound (_t)-anal_te foundin coatrol _ppt)] x 100 amountaddedCopt) Std. Coat, (_0 0 25 50 I00 2.50 500 I000 25 50 I00 250 500 I{_0 Dilotio, Facto( 10 10 t0 i0 1 l 1 I 100 I 1 1 ! 100 I I 1 ! 100 _ 1 I ! 1 tOO I 1 I 1 100 Peak An=a 5.50 8614 16102 29438 66169 142891 264459 267 659 144li 132909 239247 145872 41_,651 515606 6931 849301 826648 575640 605630 29529 13780 173871 1_.1075 355190 521363 21596 31758 2/,71389 2425189 2527002 2849870 71294 75537 307297S 3276529 2758295 3102823 77205 156964 652 940 808 34004 35258 322068 Aaalyte Fo.nd (pp0 Amount Added (pp0 Recovery (%) ND 47.6 50 95 452 500 90 8140 5000 79* 4960 5(]00 87 * 5000 * 5000 * * 100 9920 10000 57^ 591 616 * * 100 7210 1(3000 66 * 100 24200 I0000 121^ * 26200 ND ND ND 114 11900 100 10000 10(} 10000 "104A I It 119 S_ Curvc: _ (Ux wcightcd) lnmrcept = 445.057 Slope = 293.343 Cocf. OlDer, = 0.986042 C = C.mtm/sample PP = Reld fo,'6Fs_admp_ S = Sample I..CS= Labet'ato_Comrot Spike C3- C.J//bratsl_odaCrKd:=Ch_k Sumdard LP =Lab fortificdsample ND = Not deteot=i = Response betwee_ 0 aad 25 ppt NQ = Not qttantifiable= R_poe_ betwe_ 25 ppt andLOQ (50 ppt) ^Sample wu cocrected usia$ the datafound ia set 073 LO3AR. Samplet'cqukcsfuthcrdilutioa. See data set 073103AR Spreadsla_t pmpaz_ by: _1/_ " _._0_,_ sp(msm"suuiy No: F..xygeaStudyNo: A_aJyte: tons Mo_orut: Site: NA 1,.34910 PFHS 399 -> SO DecatuBr aker'sCreek RAW DATA REPORT Limit ot (_lantitatiun: Injection Vohm_: Malrix: Semp_ Volume: F_"_1Volume: _0 ppt 15 _tL Water 40.0 mL 5.0 mL SeANo: Analyst: InstnzmentType: ExtractiunDate'. A_alyzed un: 073I_A KarenRi_ _S/M$ Unit# 6 07/3b'03 08/01-02.433 Exy|m ID XC072503-.0 XClY77.,q03-1 XC072503-2 XC072503-3 XCOTL_03..4 XC072303-5 XC072503-6 _ol Wask 0106020Control 0106020 Spk A 0106020 Spk B 134910- I Spk C 1,34910-6Spk D 1,34910-12Spk E 1.34910-16Spk F XCOTLS03-1 I..34910-1 1.34910-1 Rcp 134910-4 [.34910-2 [.3491(3-3 XC072503-2 134910.6 Sponsor .3 BC2 SW4)4 BC2 SW-05 BC2 $W-06 Ouffal!to River SW-25 BC2 SW-04 BC2 SW-04 BCT.SW,O,tDup BC2 SW-04 Low Spk BC2 SW.O4HJshSpk BC2 SW-05 Se_ Code CS C3 CS CS CS CS CS C C LCS LC$ L,F LP LF LF CS $ S S FF FF CS $ Std. Run Cunc. No. (pp0 073103A- 1001 0 073103A.1C02 25 073103A-1003 073103A- I(X)4 073103A-t005 ff7I303A-I006 073I03A-I007 073103A-I008 073103A-1009 073103A-1010 073103A-IOII 073103A-1012 073103A-1013 073103A-1014 073103A-1015 073103A-|016 073103A-1017 50 100 2.50 500 I0_] 25 073103A-1018 073103A-1019 073103A- 1020 073103A-1021 073103A- 1022 50 073103A- 1023 Dilution Factor 10 10 10 10 ! ! l ! 1043 I Peak Area 0 1401 2842 5604 1313"; 26976 51345 0 0 2759 26598 30859 27946 5._454 60284 I444. 50162 49342 31968 36223 5426 2420 8666 Ana/yte Found (p_x) ND 49.7 475 5520 5(](30 * 896 882 $71 647 9730 155 Amount Added (p_X) 50 500 5_(30 5000 5000 50(]0 100 10(_0 Rccovery 4%) .* 99 95 92 97 .249+ 88 q_l_ L34910-6 Rep BC2 SW-O$ S 073103A-1024 | SSO..q 152 134910.9 BC2 $W-05 Dup S 0"/3103A-102_ .- 1 21096 377 [,34910-7 BC2 SW-05 Low Spk FF 073103A-1026 I 33965 607 1{30 452 134910.8 XC072503.3 BC2 SW-O5HighSpk FF 0'73103A-1027 I00 5342 9580 1_(300 94" C5 073103A- 1028 100 5959 I..34910-12 BC2 SW-06 S 073103A-1029 l 259042 * 134910-12 Fep BC2 SW-06 5 07310"3A-I(I30 I 237649 * 134910.15 BC2 SW-06 Dup S 073103A-1031 ! 245687 * !.,34910-13 BC2 SW-O6Low Spk FF 073103A-1032 1 275858 * 100 I..34910.14 BC2 $W-06 HighSpk FF 073103A-1033 100 9718 174(]0 10000 113A XC072503..4 CS 073103A*I034 250 14198 - L34910-16 Ou@altlo River SW-25 S 073103A-I035 I . 283517 * L34910-16 Rr.p OuffaltloRive*"SW-2_ S 073103A-1036 1 302530 * 1.34910-19 ].,349IO-17 Ouffa/ItORiver SW-25 Dup ($qtfailto River SW-25 Low Spk $ 073103A-1037 FF 0T$103A-IO3g l 276429 " 1 2";'8698 * 100 L._9!0.18 XC072503.5 Ouffallto River SW-25 High Spk FF 073103A1039 C$ 0"/3I(DA,1040 500 I00 10133 29038 18100 10(](30 104A L34910-25 1-34910-26 134910.22 EquipmentBlank.Pump EquipmentBlank.Dredge Field Co(_-ol/Fravel Blank S 073103AI041 $ 073103A,1042 $ 0731(DA-1043 1 0 ND 1 0 ND 1 0 ND 1.34910.23 FieldConrail/TraBvleanlk Low Spk FF 073 I03A-1044 I 664_ 119 100 119 L.34_910.24 Field Conu'oi/TravelBlunk HighSpk FF 073103A- 1045 100 6002 10800 10(]00 108 XC071003--6 CS 073103A.1046 1000 60941 AnalytFeound(p_t).(peaka_a. interce/pts)lutx3eDF Recove_ (%) = . [anal_e found (_ppO-_al}_tfeoundin c_atrol (p_)] x 1(}0 amount added_I_) _ :Linca(rI/xweighted) Intercept, .23.5660 Slope = 55.9970 Cool. Of DeL= 0.989093 CS = C_ib_6_ sta_u:_ LF = Lab fro'tiff-t!um'O|e S = Szmpte CK - CheckStw_ani L.C3= Laba'moo. CuntrolSpike Spreadshepetrepar_ by: / V ND = Notdctcctecl=Rcspmsebetween0and 25 ppt NQ - Not qt_ndfiable. Reqmusebctweun 2,qppt andLOQ (_0pp_) ^S;unptwas c:on_ted u._ni the(L_aafoundin set 073 I03AR. *Samplerequireslutherdilution. See datasct 073103AR. +Sampleresiduesignificantly exceedsthe s#kin I level; thcrcfot_,art_ctwa_ recoverytremor tm c_culatcd. Sq_o.mr Study No'. _yl_c_ St'_ty NO: Analyt=: Ions Monitored: Site: NA L349_0 PFOS 499 -> 99 Dccaun- Baker'sCreek RAW DATA REPORT IAmit d Qeantitafi.on: lnjecfitm Volume: MaL,_: Sample Volume: Final Vniu_e: 50plx 13 }_L Water 40.0 mL 5.0 mL Set N_c Analyst: lastnmmm Type:. E,xcactioo D_=: Analyzed ow 073103A Karma Ri_ha L,C./MS/MS Unit # 6 0'7/'31/03 08/01-02/03 EJtygea xco_m-o xc072503- l XC072503-2 XC0?2503-3 XCO'72SO3-4 _3-5 XC07_03-6 M_h,ta_i Wa._ 0106020 Control 0106020 Spk A 0106020 Spk B L34910-I Spk C L34910-6 Spk D L34910-12 Spk E I..34910-16 $pk F XCOTL_3-1 I,,,34910-1 _910-1 Rcp [.34910-4 L34910-2 L34910-3 XC072503-2 1..34910-6 1.34910.-6 Rep L34910-9 I..34910-7 1.34910-8 XC072503-3 L34910-12 L349[0-12 Rcp L349 lO-15 L,34910I3 I.,34910-14 XC_72503-4 L34910-16 L3_9 l_-I 6 _'_ I..34910-19 1.34910-17 L34910-18 XC0"/2_3-5 L34910-25 I..34910-26 L34910-22 1.34910-23 I..34910-24 XC0711D03-6 R=covery (%) ffi Sponsor - .. BC2 $W-04 BC2 SW-05 BC2 SW-06 Outfall to River SW-25 BC2 $W-04 BC2 SW-04 BC2 $W_4 Dup BC2 SW-O4 Low Spk BC2 $W-04 High Spk BC'_ SW-05 BC2 SW-0$ BC2 $W-08 D_ BC2 SW-05 Low Spk BC2 SW.05 High Spk BC2 SW-06 BC2 SW4)6 BC2 $W-(}6 Dup BC2 $W,06 Low Spk BC2 SW.,06 l'fillh Spk Outf_lI to Rivez SW-25 Ou_all to R.i.v_r_W -7.3 OUtfnil to River SW.25 Dup Oudall to Rive $W-28 Low Spk Ou_aU to Rivef SW-28 l-figh Spk Eq nipn-e.m Blank-Pua_ Eqnipnmnt Blink-Dredge P3id ControVrrave_ Blank Field Controtrrt_vl Blank Low Spk l=ield Control/rravel B lank ltigh Spk Sample cs c.s CS CS CS CS CS C C LCS LCS I._ "LI_ LF I.P C_3 $ S $ FF FF CS S S S FF FF CS $ $ $ FI: FP CS S $ S FF FF CS 5 $ S FF I_ CS $td. _ Co ne. Dilution Peak 0731m^-1001 073103A- 1002 073103A- l(X)3 073103A- 1004 073103A- 10f15 073103A- 1006 0T3tO3A-1007 073103A-I008 073103A- 1009 073103A-1010 073103A-1011 0"73103A- 1012 073 I03A-1013 073103A-1014 073103Ao1015 073103A-I016 073103A-1017 073103A-1018 073103AI019 073103A-10'20 073103A-1021 073103A- 1022 073103A- 1023 073103A- 1024 073103A-1025 073103A-1026 073103A- 10'27 073103A-102S 073103A-1029 073103A- 1030 073103A-1031 073103A- 1032 073103A-1033 073103A- 1034 073103A- 1035 _I_A-I_ 0"73103A-103"/ 073103A-I038 073103A- 1039 U73103A-IU_ 0731U3A-I041 073103A- 1042 073103A-1043 073103A-I044 073103A- 1044 U'73 IU3A.I0445 0 25 50 I00 ')_0 500 10_O 25 50 100 250 500 10_O 0 971 I963 3040 7518 17228 32298 " '0 -0 1673 15199 10 50011 10 20296 l0 96754 10 120697 954 I 280183 I 274170 I 211725 l 191631 100 6016 1656 1 44922 1 46036 1 112926 l 14_O88 I00 4333 3500 I 558236 1 571211 I 560118 1 667186 100 14981 852l l 691166 I 707270 1 656533 1 683659 100 14072 19341 I 316 1 0 1 D I 3691 1(30 3853 35665 [anal},to found _ppl-aaaiyt= found in conurol (plx)] x 100 amount added _) Anniyte Fouad Ammmt Added Rec_ve_ - . ..._: - . -. ...... "- " "_" ND 50,4 50 10l 445 500 89 * 5000 5940 5000 85 ^ * * 5000 ._ * * * " 17700 * * * " 12800 * " * 43900 " * * 41_00 100 100(30 100 100_O I00 100(]0 100 10000 62 _ l tI^ 178 '_ IO(X' biD ND ND 109 I_0 109 11400 lOGO0 114 =_Ml._ - Linear (lht Wnighta_ Iotev_pt = -56.28_0 Sloi_ = 34.2805 Cod, Of D=t. = 0.992844 C = Coau'ol utmp[e $ = Sample FF =Fleld fo_itkd semple CK = Cla:ck S_ LCS. LabOrato_. Conwol Spik_ ND .. Not demcmd=Re_4mm:btweenOand2_ I_ NQ = Not quantifi@a/e = gcape_ betw_a 25 pp tt_d LOQ (_0 ppt) ^Sample _ orrectai u._u| the data found in _q 073 i03AR. _Sampta was corrected _iag _ dam found in set 08060.3A. Sample requires _ dilutioa. Se.= data _ 073103AR. Sp_add_t _t'pan:d by: i II J spoaemr SpadyNo: Exyscn Stady No: Analytc: ions Monitored: Site: NA L34910 FOSA 498 -> 78 Decatur Baker's Creek RAW DATA REPORT Limit of l_Jantitatlon: Injection Volume: Mtu'ix: Sample Volume: Final Volume: 50ppt 15 _L Water 40.0 roL 5.0 mL Set No: Analyst: IusU'tuv.e_tType: Extraction Date: Analyzed on: 073103A Kareu Risha LC/MS/MS Unit # 6 07/31/03 08/01-02/03 Exygen Sponsor Std. Analytn Amount Sample Kua Cone. Dilution Peak Found Added Recovery tD XC072503-0 XC072503-I XC072503-2 113 Cede No. (_t) Factor Area (ppt) _pt) (%) CS 073103A-I001 0 0 CS 073103A- 1002 25 3440 CS 073103A-1003 50 6725 XC072503-3 XC072503_ CS 073103A-1004 100 CS 073I03A-I005 250 13321 31340 XC072503-5 CS 073103A-I006 500 65687 XC072503-6 Methanol Wash 0106020 Control CS 073103A-I007 10_ C 073103A- 1008 C 073103A-1009 127765 O 0 ND 0106020 Spk A LCS 073103A-1010 6872 50.6 50 101 0106020 Spk B LCS 073103A-10l I 62898 468 500 94 L34910-1 SpkC BC2 SW-04 LF 073103A-1012 10 74954 5580 5000 84^ L34910.6 Spk D BC2 SW-05 LF 073103A-1013 10 65330 4860 5000 94 L34910.12 Spk E BC2 SW-06 LF 073103A-1014 10 96556 7180 5000 95^ L349t0-16 Spk F Ottffa|l to River SW-25 LF 073 [03A-1015 10 107{)94 7970 5000 94^ XC072503.1 CS 073103A-1016 25 3545 4 L34910-1 BC2 SW-04 S 073103A-1017 I 148109 ] L34910-1 Rep BC2 SW-04 S 073103A-1018 1 143575 I L34910+4 BC2 SW-04 l_p S 073103A-1019 l 106161 790 L34910.2 L34910-3 XC072503-2 L349|0.6 BC2 SW-04 Low Spk BC2 SW-04 High Spk BC2 SW-05 FF 073103A-1020 FF 073103A-1021 CB O73103A-1022 50 $ 073103A.1023 I 90364 672 100 9716 7180 6634 1 19717 146 100 10000 -718"+ 58^ V [.349 IO-6 Rep BC2 SW-05 S 073103A-1024 I 20175 150 L34910-9 BC2 SW-05 Dup S 073103A-1025 1 52363 389 L34910-7 L34910-8 XC072503-3 BC2 SW-05 Low Spk BC2 SW-05 High Spk FF 073103A-1026 1 67031 498 104:1 352 FF 073103A-I027 100 5639 4140 100_0 40 CS 073103A-1028 100 13989 L34910-12 BCT.SW-06 S O73103A-IO29 1 269867 L349 tO- 12 Rep BC2 SW-06 S 073103A-I030 L 263411 I..34910-15 BC2 SW-O6Dup S 073103A-1031 I 276134 L34910.13 BC2 SW-06 Low Spk FF 073103A-1032 1 284082 100 L34910-14 BC2 SW-_6 High Spk FF 073 IO3A-1033 I00 11410 8440 10000 6(7" XC072503,-4 CS 073I03A-I034 250 33866 - L34910-16 Ouffall to River SW-25 S 073103A-1035 I 358032 L34910.16 Rep L34910.19 OuffaB to River BW-25 Outfall to River SW-25 Dup S 073103A-1036 S 073103A-1037 t 358872 1 369645 * L34910.17 Ouffall to River SW-25 Low Spk FF 073103A. 1038 I 311246 * 100 L34910-18 XC072503.5 Outfall to River SW-25 High Spk FF 073103A-1039 100 12191 9020 I0000 58^ CS 073103A-1040 500 72430 L34910-25 L.34910-26 L34910.22 Equipment Blank-Pump Equipmont Blank-I_,edge Field Con_ol,"Travel Blank S 073103A-1041 S 073103A.1042 S 073103A-1043 I 0 ND I 814 ND 1 0 ND L34910.23 Field Contml/Trtvel Blank LOw Spk FF 073103A- 1044 1 12140 89.8 IO0 90 L349 IO-24 XC071003-6 Field ConlroFTravel Blank High Spk FF 073103A-1045 100 16047 11900 lOOO0 119 CS 073103A-1046 1000 139302 Analyte Found (ppt) - (peak area - intercept) / slope x DF Recovery (%) - [analyte found (ppt).ana]_/tefound in coatrol _PgJx 1oo an-mauladded (ppl) $_tndardCurve : Linear (I/x weighted) Intercept = 78.1882 Slope * 134.313 Conf. Of Dot. = 0.995963 CS = Cah'brttion standard LF = Lab fortified sample CS "= SaCmonptlreotsamplo FLFC=S =FLianbtdofroa_tfotreydCsaomntprloel Spike CK = Check Standard ND _ Not detected - Response between 0 and 25 ppt V NQ = Not quantifiable - Response between 25 ppt and LOQ (50 ppt) Spreadsheet prepared by:. ,_/_ ./0,,,1_,0 _ ^Sample was corrected usm.gthe data found in set 073103AK Sample requires luther dilution. See data set 073103AR. +Sample residue significantly exceeds the spiking level; therefore, an accurate recovery cannot be calculated, i i _, n,v R E S EA R C H State College, PA 16801 Fax: 814-231-1580 SAMPLE TRANSFER SHEET Protocol Number: NA Exygen Study Number: L34910 Exygen Sample # "_ Sponsor Sample # BC2SW-04 BC2SW-04LowS' pk BC'2SW-IMHighSpk Be2 SW.-eDi -_p BC2SEIZe4 Exygen Sample # _. Sponsor Sample # BC2SW-06HighSpk _ '' I BC2SW'-06Dup _.. Ouffaltlo RiverSW-2._ .... _ c_a_ tom,=,sw.:25Lows# _ oua.U.toRivesrw-z_Hi_ spk _, --L349:0-6 - sc2sw.05 Be2 Sw-o5 LowS._k LS_Ot-O--tO_. _ 1G-Z0 _ OutfaatoRiv_.,SW-Z5Dup Outfallto RiverSW-25SED r _Anl_ o _ BC2SW-05H/_hSpk _ OuffalItoRiverSW-25SEDDUP 1 1 BC2SW.-05Dup "L349 i0-2-2-- Field Control/'r,,ravel Blank [_ao m _n BC'2SED-05 -L54_ i0-25- Field Control Low Spk BC2SEI_06 _ Field .ControlHigh Spk. _ at-'2sw-c_ _ Equipment Blank Pump BC-'2SW-06LowSpk t _ Equipment Blank:Dredge Karen Risha 7/31/03 0800 Requested By (Printed Name/Date/Time) Samples removed from: _ Samples removed from: _'_ff _ _ BOX# "-" Box# _ Shelf# "'-" Shelf# Samples transferred to the custody of _:_l_'_ Samples received from custodian; Samples moved to _ Samples removed from _ 3b Samples returned to /'_ r2aoo 53 _" Comments: _ _-- Sample Custodian Initials/Date/Time Laboratory Personnel Initials/Date/Time ce g, zle/o o 3 Sample Custodian Initials/Date/Time _I _cl (h _l"e 5 {._'_y'_O " December 19, 2002/6 c--en 3058R.Po oonvee142 _V_ R E S E A t_ C H State College, PA 16801 Fax: 814-231-1580 Internal Chain of Custody/Fortification Sheet F_,xygenStudy Number: _ Matrix: Water Sponsor Study/Protocol No: NA The samples listed below were removed from refrigerator No, _ j Time te_O Dat__ lnidals /_ CLIENT SAMPLE ID , [ na EXYGEN ID'NUIVIBER"I 0106020 Control .i VOLUME (mL) I FORT/_ICATION (ng) 40.0 na 0106020..Spk A 40.0 na 0106020 Spk B 40.0 BC2 SW-04 L34910-1 Spk C 40.0 BC2 SW-05 1,34910-6 Spk D 40.0 BC2 SW-06 L34910-12 Spk E 40.0 OutfaLlto River SW-25 L34910-16 Spk F 40.0 BC2 SW-04 L34910-1 40.0 2.0 20.0 200.0 200.0 200.0 200.0 - BC2 SW-04 BC2 SW-04 Dup L34910-1 Rep 40.0 L34910-4 40.0 . BC2 SW-04 Low Spk L34910-2 40.0 I BC2 SW-04 High Spk L34910-3 40.0 - . BC2 SW-05 L34910-6 40.0 - BC2 SW-05 L34910-6.Re p 40.0 BC2 SW-05 Dup L34910-9 40.0 BC2 SW-05 Low Spk BC2 SW-05_High Spk BC2 SW-06 L34910-.._7 40.0 L34910-8 40.0 L34910-12 40.0 BC2 SW-06 L34910-12 Rep 40.0 BC'2SW-06 Dup L34910-.!5 40.0 BC2 SW-06 Low Spk L34910-13 40.0 BC2 SW-06 High Spk L34910-14 40.0 1, ., Spiking Solution Used Volume Used for Spiking ]Initial/Date 0106020 Spk AB L34910-1Spk C L34910-6Spk D L34910-12 SpkE L349t0-16SpkF FF006611110033--12((11000aa__/m/mLL)) 200 pIxLL(200 plaLLmiecropipet) _ " I/b'"]][__],_I_ . F060203-2_1000ag/mL,) 200 I.tL(.200 I.d.m, ieropipet) _ /6"71_,'_',_ F060203-2 (1000n_/mL) 200 FL(200 IxLmicropipet) "_ 1671_16 F060203-2(1000n_/mL) 200 IAL(200 gLmicropipet) _ /0"71:_'1{_ F060203-2_1000ngmL) 200FL(200_tLmicropipetI)__/ /6"/I_11_ t/ All sampleswere measured: Time /O2-O /- Date t_'7],_/O._ [t AftermeasurinsgampleswerereturnetdorefrigeraNto?.r Time //0_) Date 0"//31/0_ It Initials Imtials /_.,,_ Comments: 200ld.. of 250 mg/mL sodium thiosu]fat= was added to all samples be.fore spiking, laitials/Dat,-: __ I li Analysis Summary: Data Set: 13"/510_ Data Set: _ Data Set: _ Initials/Date: _" Initials/Date: __"_ Initials/Date: _/___. _[_l [_,,_ Set extraction/analysis dataverifibeyd: _]Y} F Date: July26,2001/6 _//_'/_ I llll , , II I I II r.',:.,-..=,..,,-en 3os o=Phhoovnoo:8 _IV _ R E S E A R C H State College, PA 16801 Fax: 814-231-1580 Internal Chain of Custody/Fortification Sheet Exygen Study Number: L34910 Matrix: Water Sponsor Study/Protocol No: NA The samples listed below were removed from refrigerator No.,.._l_._ t Time PAID Date rY'11811_ Initials _ CL.IENT SAMPLE ID .... Outfall to River SW-25 EXYGEN ID NUMBER' _, [ VOLUME (mL) L34910016 40.0 FORTIF!CATiON (ng) .. Ou!fall to River SW-25 L34910016 Rep 40.0 Outfall to River SW-25 Dup.. L3491 0019 , 40.0 - OuffaU t9 River SW-25. Low Spk L34910-17 40.0 Ouffall to River SW-25 High Spk I.,34910-18 40-0 Field Control/Travel Blank L34910022 40.0 -. Field Control/Travel Blank Low Spk_ L34910-23 40.0 Field Control/TraveI Blab.. High Spk L34910024 40.0 Equ!pment Blank-Pump L34910025 40.0 EquiPment Blank-D.r.edse 1,349! 0026 .. 40.0 J _ -' , . ,, , .... II 1 Spiking Solution Used Volume Used for Spiking Initial/Date All samples were measured: ta TimejO2/D Date _ After measuring samples were returned to refrige.rator No. 32-- Initials Time ] 1_ Date _ I I Initials. /a_ Comments: 2ooILLof250mg/mLsodiumthiosulfamwasaddvdtoall samplebseforespikingl,nitlals/Date_: 6hA Analysis Summary: DD:::Ss::: _j_..S" Set extraction/analysis data verified by: ,[_.1,1,1,/c[ . _" i_.::_s_9_: __ Dat:e. _/__//)-_ fJul'y 26, 200116 I iii II I II Ittnt t t |I I I Ii 0 Cu i i il il _ III IIII I II (:_ @d 0 <n i ,m ._, D J n rn r_ O O tO -.. ._ c- _ _ >-co E IJ. dJ d} .C:: t- = O0 Q..O. ,= _.9.___ o_ _ IIllml II LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exygen Study No: L34910 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #6) Computer: Software: HPLC Equipment: COMPAQ Professional Workstation AP200 Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 Hewlett Packard (HP) Series 1100 I-tPBin Pump HP Autosampler I-IPVacuum Degasser HP Column Oven HPLC Column: Genesis C-8, 5 cm x 2.1 mm i.d. x 4 la (Exygen ID: 74A) (JONESCHROMATOGRAPHY: Part No. FK5962E) Mobile Phase (AB):: 2MmetMhanAoml monium Acetate in Type I Water la_00_)/01 _5 i Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 _ Phone: (814) 272-1039 FAX: (814) 231-1580 NOTE: The next 3 pages are computer generated printouts from the masslynx software Program. The pages contain the instrument settings used for the analysis of this data set. AU Handwritten Peak ID' s by: _b-_Ib_ i ii %_m_ Scanning Method Method: Last Modified: Report C:kMASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\C6 Thu Jul 31 16:23:50 2003 C8 SULF C8 ACID PFOSA Page 1 Printed: Solvent Delay Fri Aug 01 08:36:30 2003 ( mins ) : 0.00 _I0,I _ Analog Channel Function :1 4 : unused MRMof 4 Mess Pairs ( ESP- ) Inter Channel Delay ( Secs ) : Span ( Daltons ) : Start Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 12.00 1 Dwell (Secs) Coll Energy (eV) Cone ( V 1 399.00 80.00 0.20 35 50 2 413.00 369.00 0.20 10 10 3 498.00 78.00 0.20 30 50 4 499.00 99.00 0.20 40 30 4 q_ Method Report Method File: Last Modified: c:\masslynx\fluorochemicals.pro\acqudh\pfh, Friday, Augllst 01, 2003 08_27:00 water Page 1 ,_ Printed: Friday, August 01, 2003 08:36:39 _I_ HPII00 LC Pump Initial Solvents A% B% C% D% Conditions 90.0 I0.0 0.0 0.0 Flow Stop Min Max Oven Oven (ml/min) Time (mins) Pressure (bar) _ressure (bar) Temperature Left(0C) Temperature Right(C) 0.300 20.0 0 400 35.0 35.0 HPII00 LC Pump Gradient Timetable The gradient Timetable contains 8 entries which are : Time A% B% C% D% Flow Pressure 0.00 90.0 i0.0 0.0 0.0 0.300 400 : 2.00 90.0 i0.0 0.0 0.0 0 300 400 | ! 5.00 9.00 i0.0 i0.0 90.0 90.0 0.0 0.0 0 300 400 0.0 0.0 0 300 400 9.50 0.0 100.0 0.0 0.0 0 300 400 14.00 0.0 I00.0 0.0 0.0 0 300 400 14.50 90.0 i0.0 0.0 0.0 0 300 400 20.00 90.0 i0.0 0.0 0.0 0 300 400 HPII00 LC Pump External Event Timetable The Timetable contains 6 entries which are : Time Initial 0.00 0.05 0.I0 11.90 12.00 Column Switch Off Off Off Off Off Off Contactl Off On O Off Off Off Contact2 Off Off Off On Off Off Contact3 Off Off Off Off On Off Contact4 Off Off Off Off Off Off HPII00 Autosampler Initial Draw Speed Eject Speed (_i/min) Draw Position (mm) Stop Time (mins) Injection Volume(_l) vial Number Conditions 200.0 200 0.50 20.00 15.0 69 _J Tuning Method Method: Report C : \MASSLYNX\FLUOROCHEMICALS. Printed: Fri Aug 01 08:37:00 2003 PRO\ACQUDB\FLUOROCHEMS _I0)I_ I_ ,I It_-S" Page 1 Dau 395.00 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Desolvation Temp. Temp. Pressures Analyser Gas Cell Vacuum Set 3.00 20 0.0 0.0 0.0 I00 300 Rdbk -2.93 -21 i00 299 Rdbk OFF 3.4e-3 Analyser LM Res 1 HM Res 1 IEnergy I 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 12 " 15 14 2 16 14.0 14.0 2.0 650 -648 Rdbk 131.4 754.2 Quantify Calibration Report Study No.:L34910, Set No.:073103A, Ext.Date:07131/03, Analyst:K.Risha Calibration: P:\Data\LCMSMS6\Mass13rnx\Fluoroohemicals.PRO\CurveDB\073103A Printed: Sun Aug 03 07:19:26 2003 Compound 1 name: C8 Acid (PFOA) Coefficient of Determination: 0.986042 Calibration curve: 293.343 * x + 445.057 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: l/x, Axis trans: None 3.22e5- Page 1 Decatur BC x xi Response- 0 ..... 0.0 , .... , .... 200.0 , .... , ..... i... ,"_ .... 400.0 600.0 , .... , .... 800.0 , .... ,ng/L 1000.0 E_Tgen Research, 3058 Research Drive, State College, PA 16801 Quantify Calibration Report Study No.=L34910, Set No.:073103A, Ext.Date:07151/03, Analyst:K.Risha Calibration: Last modified: Printed= P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\073103A Sun Aug 03 07:12:46 2003 Sun Aug 03 07:19:26 2003 !Compound2 name: C6 Sulfonate (PFHS) Coefficient of Determination:0.989093 Calibration curve: 55.9970 * x + -23.5660 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: l/x, Axis trans: None 6.09e4- Page 2 Decatur BC x Response -23.6 0.0 200.0 400.0 600.0 Exygen Research, 3058 Research Drive, State College, PA 16801 800.0 ,ng/L 1000.0 Quantify Calibration Report %_ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Calibration: Last modified: Printed: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\073103A Su31 Aug 03 07:12:46 2003 Sun Aug 03 07:19=26 2003 Compound3 name: C8 Sulfonate (PFOS) Coefficient of Determination:0.992844 Calibration curve: 34.2805 * x + 56.2500 Responsetype: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: l/x, Axis trans: None 3.57e4- Page 3 Decatur BC x x 1 Response- V 0 . ,'',, 0.0 .... ,, .". , i .... i .... 200.0 400.0 _ .... , .... 600.0 , .... t .... 800.0 _ .... i ng/L 1000.0 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Calibration Report Study No.:L34910, Set NO.:073103A, Ext.Date:07/31/03, A_alyst:K.Risha Calibration: Last modified= Printed: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\073103A Sun Aug 03 07:12:46 2003 Sun Aug 03 07:19:26 2003 Compound 4 name: PFOSA Coefficient of Determination:0.995963 Calibration curve: 134.313 * x + 78.1882 Responsetype: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: l/x. Axis trans: None 1.39e5- Page 4 Decatur BC x Response- V 0 .... 0,0 i ' "' ' _ .... 200,0 i .... _ .... 400,0 i ' ' ' ' b .... 600,0 i .... i .... 800.0 I .... _ng/L 1000,0 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, ReDort Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 1 Sample List: Last modified: Method: Last modified: Job Code: Printed: P:\Data\LCMSMS6\Massllrnx\Fluorochemicals. Sun Aug 03 07:08:13 2003 PRO\SampleDB\073103A Decatur BC P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur BC 080103 Su_ Aug 03 07:11:59 2003 Sun Aug 03 07:19:29 2003 ,}_ h_ia__ D=e c_ 5 Io%}o Run#07%;O_A_;_,To^_=,^=L_,_,,F_._,.. Name: 073103A-I001 Text : i: C8 Acid (PFOA) XC072503-0, 0 n_L Standard 073103A-1001 Sm (Mn, 2x3) 100] A J [/ 01-Aug-2003 09:24:14 LC/MS/MS #6 MRM of 4 Channels ES413 > 369 1.22e4 9.14 Area : " ' ' ' I ' ' ' ' I ' ' ' ' _I -''_-' _'_-' I ' ' ' ' 1 ' ' ' ' _I ' ' ' ' I ' ' ' ' I ' ' ' ' I ' ' ' ' I ' ' ' ' I' ' ' ' ' 1 Time 2.00 4.00 6.00 8.00 10.00 12.00 : C6 Sulfonate (PFHS) XC072503-0, 0 ng/L Standard 01-Aug-2003 09:24:14 073103A-1001 Sm (Mn, 2x3) 100] 0.8.9 1.27 212 298 454 " 478 549 MRM of 4LCCh/MaSnn/MeSlsE#S6- 8.98 9.53 .... 399 > 80 . f_ . A 998 11.16._'_ 566 80_ " ]_l----_ ''I----V ] - v 7 2.00 4.00 3:C8 Sulfonate (PFOS) XC072503-0, 0 n_i Standard 073103A-1001 Sm (Mn, 2x3) 10" 1.27 - _ 6.00 ; - V I] _ _ ' 8.00 ' ' 10.00 ,Time 12.00 01-Aug-2003 09:24:14 ./J LC/MS/MS #(_ _/ MRM of 4 ChannelsES- 9.27 11.5 499 > 9g -, ............................................... Time _1_ 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha San_ple Lilt: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Deoatur Sun Aug 03 07:11z59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 2 Decatur BC BC 080103 Name- 073103A-I001 Text : 4 : PFOSA XC072503-0, 0 ng/L Standard 073103A-1001 Sm (Mn, 2x3) 1007 4 124 37 7.14 01-Aug-2003 09:24:14 _ RM of 4LCh/ManSn/NelSs E#S69.88 .... 11.64498 > 78 /i1 , _ ,...... _) i - - _,_,o i ' " " ' I .... I'''' 2.00 I .... I ' ' ' ' I ' ' ' ' I .... 4.00 6.00 I .... I ' ' "" I ' ' ' ' I .... 8.00 10.00 I .... 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study NO.:L34910, Report Set No.:073103A, Ext.Date:07/31/03, Analyat:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 3 Decatur BC BC 080103 Name: 073103A-I002 Text : 1:C8 Acid (PFOA) XC072503-I, 25 ng]L Standard 073103A-1002 Sm (Mn, 2x3) ot 1003 8691.146- 01-Aug-2003 09:45:57 LC/MS/MS #6 MRM of 4 ChannelsES- 4135>.363e649 Area .... i .... _ ' ' 'r I _ _1 I' _ 'l '1 '' I '; T _ I''' 'l ' I" I I l ' T i_l 2.00 4.00 6.00 8.00 k ' ,- . , .... 10.00 , :-T.,--_.,j Time 12.00 _ 2:C6 Sulfonate (PFHS) XC072503-1, 25 ng/L Standard 073103A-1002 Sm (Mn, 2x3) 100 6.99 1401-_ 01-Aug-2003 09:45:57 LC/MS/MS #6 MRM of4 ChannelsES399 > 80 8.90e3 % - , .-, . , , , , , , , ...... C _' T } , ' '"" [ , ' _ ' 2.00 4.00 6.00 3:C8 Sulfbnate (PFOS) XC072503-1, 25 ng/L Standard 073103A-1002 Sm (Mn, 2x3) , , k ' I I : ' .... 8.00 ' .... 10.00 i .... TArea ' ime 12.00 01-Aug-2003 09:45:57 LC/MS/MS #6 MRM of 4 Channels ES- 9.26 499 > 99 Area ,/o 11_ , .... , .... , .... ,,..._-_T-_, ..., .... ,... 971, 1 , ...,., ._-_-.,6T.3im0ee3 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 4 Decatur BC BC 080103 Name: 073103A-I002 Text : 4 : PFOSA XC072503-1, 25 ng/L Standard 073103A-1002 Sm (Mn, 2x3) 01-Aug-2003 09:45:57 LC/MS/MS #6 MRM of 4 ChannelsES- 9.88 498 > 78 11/1 . 3440_- L._ 1.94e4Area ! 0"" .... , .... i .... , .... , .... ,...,,''', , .... , .... , ..... --,....-'LTime 2.00 4.00 6.00 8.00 10.00 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantfy Sample Report _ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified= Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07=08=13 2003 P:\Data\LCMSMS6kMasslynxkFluorochemicals.PRO\MathDBkDecatur Sun Aug 03 07:11:59 2003 Printed= Sun Aug 03 07:19=29 2003 Page 5 Decatur BC BC 080103 Name: 073103A-I003 Text : i: C8 Acid (9FOA) XC072503-2, 50 ng/L Standard 073103A-1003 Srn (Mn, 2x3) 01-Aug-2003 10:07:44 LC/MS/MS #6 MRM of 4 ChannelsES- 9.15 413 > 369 0 , _ ._,'_,.. , , . , e j ,., , '"l '" ' ', ', .... , ," ' , ' , .... , .... 2.00 4.00 6.00 8.00 , .... , . , ,-.", , . cT,Time 10.00 12.00 %_ 2:C6 Sulfonate (PFHS) XC072503-2, 50 ng/h Standard 073103A-1003Sm (Mn, 2x3) 01-Aug-2003 10:07:44 LC/MS/MS #6 MRM of4 ChannelsES- 8.99 399 > 80 ,_T-',_) .... _ T ,.,,.'1 .... I .... 2.00 4.00 3:C8 Sulfonate (PFOS) XC072503-2, 50 ng/h Standard 073103A-1003 Sm (Mn, 2x3) I'' ' :' I ' T_ , I " ' "-" i .... 6.00 8.00 1 " ' _" I ' " _ ';'T" ' ' _ i Time 10.00 12.00 01-Aug-2003 10:07:44 LC/MS/MS #6 MRM of 4 ChannelsES- 9.26 499 > 99 'o/1 0_ .... , .... ,,..,., 2.00 .... , .... 4.00 , .... , .... 6.00 ,, ,-,..., .... 8.00 _,,__....., .... 10.00 ,,-.,..-, ,TiAmreea 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 llm_ Quantify Sample Study No.:L34910, Report Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\L_MSMS6\Masslynx\Fluorochemicals.PRO\Saur_leDB\O73103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 6 Decatur BC BC 080103 Name: 073103A-I003 Text : 4 : PFOSA XC072503-2, 50 ng/L Standard 073103A-1003 Sm (Mn, 2x3) 10o_0 01-Aug-2003 10:07:44 LC/MS/MS #6 MRM of 4 Channels ES- 6725- 3.68e4 Area 9.89 498 > 78 ! ,'_ , , _ . . ,, , .... 2.00 } .... _ .... 4.00 , . . .-. _, . .',l .... , .... 6.00 8.00 , . :- .... . ,. ,-- .,Time 0.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify sample Report %_ Study No.:L54910, Set No.:073103A, Ext.Datm:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code : P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Stul Aug 03 07:08:13 2003 P :\Data\LCMSMS6kMasslynxkFluorochemicals. PRO\MethDB\Decatur S_ Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 7 Decatur BC BC 080103 Name: 073103A-I004 Text : i: C8 Acid (PFOA) _ :_..,._.-- XC072503-3, 100 ng/L Staiidard " 073103A-1004 Sm (Mn,2x3) 01-Aug-2003 10:29:31 LC/MS/MS #6 MRM of 4 ChannelsES- 9.15 413 > 369 10(3% ..................... 2.00 4.00 _ 2:C6 Sulfonate (PFHS) XC072503-3, 100 ng/L Standard 073103A-1004 Sm (Mn, 2x3) 6.00 294381 1.81e5Area 1 _ _ , . . _ .... _ Time 8.00 10.00 12.00 01-Aug-2003 10:29:31 LC/MS/MS #6 MRM of 4 ChannelsES- 9.01 399 > 80 lql/1 O' . . ,_ .... , , ,.. 2.00 , .... , .... 4.00 , .... , .... 6.00 56041 3.44e4Area , .... i .... , , . . -, . , ... , .... ,Time 8.00 10.00 12.00 3:C8 Sulfonate (PFOS) XC072503-3, 100 ng/L Standard 01-Aug-2003 10:29i31 LC/MS/MS #6 073103A-1004 Sm (Mn, 2x3) 9.26 MRM of 4 Chan4n9e9ls>ES99- 0'; ,, , , .-:': ,'. , .... , , . . , .... oo[ 9e -, : , _ . , ,- ,, r, , . :-7", , , , _ , , . . . ,Time V 2.00 4.00 6.00 8.00 10.00 12.00 Faygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %_ Study No.:L34910, Set No._073103A, Ext.Date:07/31/03, Analyst_K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LC_SMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07=Ii:59 2003 Printed: Sun Aug 03 07=19:29 2003 Page 8 Decatur BC BC 080103 Name: 073103A-I00_ Text : 4 : PFOSA XC072503-3, 100 ng/L Standard: 073103A-1004Sm(Mn,2x3) 01-Aug-2003 10:29:31 LC/MS/MS #6 MRMof4 ChannelsES- 13321 7.20e4 Area -" 0', . .,, .... , .... 2.00 _.... , .... , .... F',.,, 4.00 6.00 _.... ', .... 8.00 L ',, ...... 10.00 , .... ,Time 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.=073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified= Job Code= P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 Pz\Data\LC_SMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur SIM_ Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 9 Decatur BC BC 080103 Name: 073103A-I005 Text : i: C8 Acid (PFOA) XC072503-4, 250 n_L Standard 073103A-1005 Sm (Mn, 2x3) 10(_ . ." 9.15 _ 66169 01-Aug-2003 10:51:16 LC/MS/MS #6i MRM of 4 ChannelsES-' 413 > 369 4.06e5 Area C .,,,, ,_'_., , , .... 2.00 , .... , .'_.-_ r .... , .... 4.00 6.00 %_# 2:C6 Sulfonate (PFHS) XC072503-4, 250 ng/L Standard 073103A-1005 Sm (Mn, 2x3) _ .... ", ....... 8.00 8.99 ",, _., ,, ,.., ,Time 10.00 12.00 01-Aug-2003 10:51:16 LC/MS/MS #6 MRM of 4 ChannelsES399 > 8(3 11/1 O r .... , .... , .... 2.00 , .... _ .... ', .... -, .... 4.00 6.00 3:C8 Sulfonate (gFOS) XC072503-4, 250 ng/L Standard 073103A-1005 Sm (Mn, 2x3) IL, , , , ,-. , , _.... 2.00 "'_,', , , , .... 4.00 , .... , .... 6.00 13137, .... , ...... 8.00 ". , , .... 10.00 8.10e4Area , .... ,Time 12.00 01-Aug-2003 10:51:16 LC/MS/MS #6 MRM of 4 ChannelsES- 9.25 499 > 99 , .... , .... 8.00 1_ .... T , .'. ,i .... Area ,Time 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _mJ Study No.:L34910, Set No.:073103A, Eat.Date:07/31/03, Analyst:K.Risha Sam_ie List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Suux Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: SunAug 03 07:19:29 2003 Page i0 Decatur BC BC 080103 Name: Text: 073103A-I005 4: PFOSA XC072503-4, 250 ng/L Standard 073103A-1005 Sm (Mn, 2x31 01-Aug-2003 10:51:16 LC/MS/MS #6 MRM of 4 ChannelsES- 31340- 1.69e5 Area 01 .... _ .... , .... 2.00 , .... _ .... 4.00 , .... , .... 6.00 _ . . .. , .... 8.00 , ....... 10.00 , . , ,, ,Time 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha San_le List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\San_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MathDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page ii Decatur BC BC 080103 Name: 073103A-I006 Text : 1:C8 Acid (9FOA) XC072503-5, 500 n_L Standard 073103A-1006 Sm (Mn, 2x3) 1_,_ 9.13 142891- 01-Aug-2003 11:12:56 LC/MS/MS #6 MRM of 4 ChannelsES413 > 369 8.51e6 Area ''' I '_t' ' ' I .... 2.00 I .... I ' ''' ' l .... I ' ' ' ' I ' "'' ' ['"" ' ' ' ' r ' ' I .... 4.00 6.00 8.00 10.00 , ' ,,,1Time 12.00 V 2:C6 Sulfonate (PFHS) XC072503-5, 500 ng/L Standard 073103A-1006 Sm (Mn, 2x3) 01-Aug-2003 11:12:56 LC/MS/MS #6 MRM of 4 ChannelsES- 8.99 399 > 80 1Io/! 0 I .... , .... , .... 2.00 , .... _ .... 4.00 3:C8 Sulfonate (PFOS) X0072503-5, 500 ng/L Standard 073103A-1006 Sm (Mn,2x3) , .... _ .... 6.00 26976 1 _ .... , .... , .... , .... 8.00 10.00 1.64e5Area , .... ,Time 12.00 01-Aug-2003 11:12:56 LC/MS/MS #6 MRM of 4 ChannelsES- 9.25 499 > 99 Area i 0 t .... _ ,",,,, .... 2.00 , .... , .... 4.00 , .... , .... 6.00 , .... , .... 8.00 ', .... , .... 10.00 , .... ,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify sample Study No.:L34910, Report Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslyr_\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 12 Decatur BC BC 080103 Name: 073103A-I006 Text : 4 : PFOSA XC072503-5, 500 ng/L Standard 073103A-1006 Sm (Mn, 2x3) 11_ 01-Aug-2003 11:12:56 LC/MS/MS #6 MRM of 4 ChannelsES- 9.90 498 78 65687- Area 3.53e5 ,'. ,., .... _ .... 2.00 _ .... , .... 4.00 t .... i .... 6.00 , .... _', ,', , b ....... 8.00 10.00 '[ .... ,Time 12.00 Ex1_en Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:073103A, Ext.Date:07131/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 13 Decatur BC BC 080103 Name: 073103A-I007 Text : i: C8 Acid (PFOA) XC072503-6, 1000 n_L Standard 073103A-1007 Sm (Mn, 2x3) 01-Aug-2003 11:34:42 LC/MS/MS #6 MRM of 4 ChannelsES- 9.13 413 > 369 110_ 264459- 1.57e6Area i , . . . , .... ,',. , . r .... , .... 2.00 4.00 , .... , .... 6.00 , .... ," ' ..... 8.00 _ 2:C6 Sulfonate (PFHS) XC072503-6, 1000 ng/h Standard 073103A-1007 Sm (Mn, 2x3) 8.97 , .... 10.00 , .... ,Time 12.00 01-Aug-2003 11:34:42 LC/MS/MS #6 MRM of 4 ChannelsES399 > 80 Area 110o_ ....T _.... , .... _.... ,.... ,.... ,.... , .... ,5.1.3.4.51, ....-.,.... j.. .;,3T.1i4mee5 2.00 4.00 6.00 8.00 10.00 12.00 3:C8 Sulfonate (PFOS) XC072503-6, 1000 ng/L Standard 073103A-1007 Sm (Mn, 2x3) 01-Aug-2003 11:34:42_ LC/MS/MS #6 I MRM of 4 ChannelsES- l 9.25 499 > 99I Area 1 .... , .... f .... , .... , .... , .... , .... , .... , .... , .... ,., ,. _ .... _Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.zL34910, Re_ort Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 14 Decatur BC BC 080103 Name: 073103A-I007 Text : 4 : PFOSA XC072503-6, I000 n_L Standard 073103A-1007 Sm (Mn,2x3) 1(0--_ 01-Aug-2003 11:34:42 LC/MS/MS #6 MRM of 4 ChannelsES- 9.91 498 > 78 127765" 6.:79e5 Area i 0 j .... , .... , .... 2.00 , .... , .... 4.00 , .... , .... 6.00 , .... , .... 8.00 , ....... 10.00 ,..., ,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\MethDB\Decatur Su_ Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 15 Decatur BC BC 080103 Name: 073103A-I008 Text : i: C8 Acid (PFOA) Methanol Wash 073103A-1008 Sm (Mn, 2x3) 9.13 01-Aug-2003 11:56:30 LC/MS/MS #6 MRM of 4 ChannelsES413 > 369 A __ ,_ Area 0." ._' ' '"'....I...'..' ' J ' ' ' ' I " ' ' ' 1"' ' ' ' I '"' 2.00 4.00 ' ' I ' ' ' ' I" 6.00 " ' ' I ' ' ' ' '1 .... 8.00 I .... 10.00 I ' r', , I Time 12.00 ql_ 2:C6 Sulfonate (PFHS) Methanol Wash 01-Aug-2003 11:56:30 073103A-1008 Sm (Mn, 2x3) 'oo7 MRM of 4LCh/MaSnn/MeSlsES#6- %_ .... =_"" 2.7_'.4U .... /.Ub _kv/_ - 0_;... , . . .., .... ", .... , . . i _ .... i .... , .... , .... _'.... _ .... { .... _Time 2.00 4.00 6.00 8.00 10.00 12.00 3:C8 Sulfonate Methanol Wash (PFOS) 01-Aug-2003 11:56:30 073103A-1008 Sm (Mn, 2x3) 10_- MRM of 4LCCh/MaSnn/MelSsE#S6- 9.27 499 > 99i vl 0-24 0.86 2.58 3424004.7,5.02 724750 8:,59 A 9"59 10A84 11"6_7 933 .... L/,L 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modifiedz Job Code: P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Su_ Aug 03 07:19:29 2003 Page 18 Decatur BC BC 080103 Name: 073103A-I008 Text : 4 : PFOSA Methanol Wash 073103A-1008Sm (Mn, 2x3) 100-1/0.12 J/_ 3 46 5.62 | ,_-Aug-2003 11:56:3C LC/MS/MS#6 MRM of 4 ChannelsES- 9 "90 498 > 78 /\ 909 % 0.89 175 229 297 i 397 4.63 6.13 6.76 7_3 8.99..9.22 // 10.58 11 64 i 0 _ ' ' ' ' |''- ''' I''' ' )' 2.00 '''] '' ''I' 4.00 ' ' ' I ' ' ' ' I ' ' ' ' I ' '" 6.00 8.00 ' ' I ' ' ' ' [ ' _- ' ' t' ' ' ' ' 1 Time 10.00 12.00 V EXygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _mJ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List= Last modified: Method= Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\Sa_pleDB\073103A Sun Aug 03 07:08:13 2003 P:\DatakLCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07=11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 17 Decatur BC BC 080103 Name= 073103A-I009 Text : i: C8 Acid (PFOA) 0106020 Control 073103A-1009 Sm (Mn, 2x3) " 01-Aug-2003 12:18:08 LC/MS/MS #6 MRM of 4 ChannelsES- i 9.15 llo/1 /N__ /___ ...... 0 r, 7_',. .,....... , ,'TC,-7,,_ , 2.00 4.00 "-;,-TT,. -:-, ..., .... 6.00 659 413>3691.72e4Area ,.... ,.... , .... ,.... ,Time 8.00 10.00 12.00 %_ 2:C6 Sulfonate (PFHS) 0106020 Control 073103A-1009 Sm (Mn, 2x3) 10n-` 0.89 _ ,,_ 0.20 2 4.06 386A422 01-Aug-2003 12:18:08 | LC/MS/MS #6 .I, MRM of4 ChannelsES- _J 10.421155399 > 80 8p lO.24A. ", O/o._U _ - - _-_-----_F _ _ -_ _ v-_ - -_--_,- ,., - _- . .... , .... ,.... , .... , .... ,.... ,.... , .... ,.... ,.... , .... , .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 3:C8 Sulfonate (PFOS) 0106020 Control 073103A-1009 Sm (Mn, 2x3) 1,_,__0.41 uu_ A 1 29 01-Aug-2003 12:18:08 ! LC/MS/MS #6 ,I MRM of 4 ChannelsES499 > 99 9.25 1.02e3 O/,o_/ .... " 2.86 ,.... , .... 2.00 ,.... , .... 4.00 , .... , .... 6.00 ,.... , .... 8.00 10.41 7 ,.... , .... 10.00 , .... ,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.=L3&910, Report Set No.:073103A, Ext.Date=07/31/03, Analyst:K.Risha Sample List= Last modified: Method: Last modified: Job Code: P:\Data\LCMS_S6\Massllrnx\Fluorochemicale.PRO\Sam_leDB\073103A Sun Aug 03 07:08=13 2003 P=\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: S_n Aug 03 07:19:29 2003 Page 18 Decatur BC BC 080103 Name: 073103A-I009 Text : 4 : PFOSA 0106020 Control 073103A-1009 Sm (Mn, 2x3) 100-1 2.11 _ 4.20 4_38.50 01-Aug-2003 12:18:0E RM of 4 ChannelsESLC/MS4/M98S >-7#8e! 9.96 11.18 11.63 684 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 *_iJ Quantify Sample Study No.:L34910, Report Set No.:073103A, Ext.Date:07131103, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:kData\LCMSMS6\Masslynx\Flucrochemicals.PRO\Sam_leDBk073103A Sun Aug 03 07:08:13 2003 P:kData\LCMSMS6kMasslynxkFluorochemicals. PROkMethDBkDecatur Sun Aug 03 07:11=59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 19 Decatur BC BC 080103 Name: 073103A-I010 Text : 1:C8 Acid (PFOA) 0106020 Spk A, 50 ng_ 073i 03A-1010 Sm (Mn, 2x3) 01-Aug-2003 12:39:57 LC/MS/MS #6 9.15 MRM of 4 Cha4n1n3el>sE36S9- 10C% 144111 8.95e4Are_ i C _ ...... , , ,, i-, ,-,, , , ,, , , .... , ,:, , ,?,_ , ,, , , , ,.... , , , ,-,',', , , ,-,Time 2.00 4.00 6.00 8.00 10.00 12.00 _ 2:C6 Sulfona_e (PFHS) 0106020 Spk A, 50 ng/L 073103A-1010 Sm (Mn, 2x3) 01-Aug-2003 12:39:57 LC/MS/MS #6 MRM of 4 ChannelsES- 8.99 399 > 80 111/1 0u, .., .... , .... 2.00 , .... , .... 4.00 3:C8 Sulfonate (PFOS) 0106020 Spk A, 50 ng/L 073103A-1010 Sm (Mn, 2x3) i .... , .... 6.00 27591 , . . , .... _..' 8.00 . , .... 10.00 1.73e4Are_ , .... ,Time 12.00 01-Aug-2003 12:39:57 LC/MS/MS #6 MRM of4 ChannelsES- 9.27 499 99 1,1/1 1673] 1.08e4 0-.r"."_'-_;-f7_.-.. _ .... , .... , .... , . . . . , .... , .... i ........ ___._Are,a.... = .... I lime ; 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify SaE_le ReDort _,_ Study NO.:L34910, Set No.:073103A, Ext.Date:07131/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P=\Da_a\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07=08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Su_ Aug 03 07:19:29 2003 Page 20 Decatur BC BC 080103 Name= 073103A-I010 Text : 4 : PFOSA 0106020 Spk A, 50 ng/L 073103A-1010 Sm (Mn, 2x3) 01-Aug-2003 12:39:57_ LC/MS/MS #6I MRM of 4 ChannelsES- I 9.89 498 > 781 1Ci/1 6872- 3.70e41Are_ 1 0', ,. , .... , .... ,, ,.,,,, .... , .... , .... , .... ,,.,,..,, .- .... ,, r.,,, ,Time 2.00 4.00 6.00 8.00 10.00 12.00 %ol _gen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/O3, Analyst:K.Risha Sample List: Last modiEied: Method: Last modified: Job Code: P:\Data\LCMSMS6\MasslynxkFluorochemicals.PROkSam_leDBk073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Deoatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 21 Decatur BC BC 080103 Name: 073103A-1011 Text: i: C8 Acid (PFOA) 0106020 Spk B, 500 ng/L 073103A-1011Sm (Mn, 2x3) 10 . ." . 132909- 01-Aug-2003 13:01:43 LC/MS/MS #6 MRM of 4 ChannelsES- 7.82e5 Area 0' .... ,_"_.,. ,'.., 2.00 ,.,.., . . , . , .... J .... 4.00 6.00 2:C6 Sulfonate (PFHS) 0106020 Spk B, 500 ng/L 073103A-1011 Sm (Mn, 2x3) 1C _ .... , ....... 8.00 2659 , .... 10.00 , .... ,Time 12.00 01-Aug-2003 13:01:43 LC/MS/MS #6 MRM of 4 ChannelsES- 1.54e5 Area i 8.9_ 399 > 80 2.00 4.00 6.00 8.00 10.00 12.00 3:C8 Sulfonate (PFOS) 0106020 Spk B, 500 n_t 073103A-1011 Sm (Mn, 2x3) 01-Aug-2003 13:01:43 LC/MS/MS #6 MRM of4 ChannelsES- 927 499 > 99 Area ! .... , .... , .... , .... , .... , .... , .... , .... , .... , .... i .... ,,, ,'. ,Time 2.00 4.00 6.00 8.00 10.00 12.00 Ex1_en Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:073103A, Ext.Date=07/31103, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\MasslyIIx\Fluorochemicals.PRO\Sam_IeDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluoroohemicals.PRO\MethDB\Deca_ur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 22 Decatur BC BC 080103 Name: 073103A-I011 Text : 4 : PFOSA 0106020 Spk B, 500 ng/L 073103A-1011Sm (Mnl 2x3) 01-Aug-2003 13:01:43 LC/MS/MS #6 MRM of 4 ChannelsES- 9.90 498 > 78 1i0-_ 628981 3.29e5Area, i .... , .... , .... _ .... '_ .... _ .... _ ..... _ .... _ ,'",', , _ .... _ .... _ .... _Time 2.00 4.00 6.00 8.00 10.00 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Qu_zltify Sample ReDort Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified= Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Dacatur Su_ Aug 03 07=11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Pa_e 23 Decatur BC BC 080103 Name: 073103A-I012 Text : i: C8 Acid (PFOA) L34910-1 Spk C, 5000 ng/L, DF=10 073103A-1012 Sm (Mn, 2x3) 01-Aug-2003 13:23:31i LC/MS/MS #6 MRM of 4 ChannelsES- 9.14 413 > 369i 0' .... J_"_,,,,,, ,",, .... , .... 2.00 4.00 ql_ 2:C6 Sulonate (PFHS_ L34910-1 Spk C, 5000 ng/h, DF=10 073103A-1012Sm (Mn, 2x3) 1 _ .... , .... 6.00 ,L , .... , ........ 8.00 , .... 10.00 , .... ,Time 12.00 3085 01-Aug-2003 13:23:31 LC/MS/MS #6 MRM of 4 ChannelsES-: 1.84a5 Area 0o0_-.... , .... , .... 2.00 , .... , .... 4.00 3:C8 Sulfonate (PFOS) rL34910-1 Spk C, 5000 rig/L, DF=10 073103A-1012Sm (Mn, 2x3) , .... , .... 6.00 , .... , 8.9%1_ ' ' "_ .... 8.00 10.00 v .... 39,T9im> 8e0 12.00 50011 01-Aug-2003 13:23:31 LC/MS/MS #_ MRM of4 ChannelsES- 2.91e5 Area 110__ ii I .... _ .... , .... , .... _ .... ,.... _,,,,, 9.271 499 > 99 .... _..,,, .... _ .... _ .... _Time V 2.00 4.00 6.00 8.00 10.00 12.00 _xygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Re_ort Set No.=073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified= Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Su_ Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 24 Decatur BC BC 080103 Name: 073103A-I012 Text : 4 : PFOSA L34910-I Spk C, 5000 n_t, DF=I0 073103A-1012Sm (Mn, 2x3) 01-Aug-2003 13:23:31 LC/MS/MS #E MRM of 4 ChannelsES-! 74954 4.01e5 Area Jt .... _', , , _ .... _ .... _ .... _ .... , .... _ , ,', , _ ,, , , _ ....... 2.00 4.00 6.00 8.00 10.00 , , , ,, ,Time 12.00 Exygan Research, 3058 ResearQh Drive, State College, PA 16801 Quantify Sample Report R_ Study No.:L34910, Set No.:073103A, Ext.Date:07/31103, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code : P:\DatakLCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P :\Data\LCMSMS6\Massly_x\Fluorochemicals. PROkMethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 25 Decatur BC BC 080103 Name: Text 073103A-I013 i: C8 Acid {PFOA) L34910-6 Spk D, 5000 n_L, DF=10 073103A-1013 Sm (Mn, 2x3) 1^,_ 9.13 145872- 01-Aug-2003 13:45:17 LC/MS/MS #6 MRM of 4 ChannelsES413 > 369 8.79e5 Area j .... -i_.,._ .... 2.00 _ .... _ .... 4.00 _q_# 2:C6 Sulfonate (PFHS) 534910-6 Spk D, 5000 ng/L, DF=10 073103A-1013Sm (Mn, 2x3) ,.,',,, .... 6.00 _ .... ', .... 8.00 _ , , ,'_ .... 10.00 _ .... _Time 12.00 01-Aug-2003 13:45:17 LC/MS/MS #6 MRM of 4 ChannelsES- 8.98 399 > 80 111/l 0 I .... _ .... i .'".,., 2.00 .... , .... 4.00 3:C8 Sulfonate (PFOS) L34910-6 Spk D, 5000 ng/L, DF=10 073103A-1013 Sm (Mn, 2x3) i".... _ .... 6.00 279461 i .... , .... , .... , . ,-.., 8.00 10.00 1.64e5Area .... _Time 12.00 01-Aug-2003 13:45:17J LC/MS/MS #6 I MRM of 4 Channels ES- I 9.25 499 > 99I Area 0' .... _- .... , '', ' , .... r..,, _ .... , .... , .... .... , .... i".,,,, .... ,Time V 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify sample Study No.:L34910, Report Set No.:073103A, Ext.Date:07/31103, Analyst=K.Risha Sample List= Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslymx\Fluorochemlcals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07=11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 26 Decatur BC BC 080103 Name: 073103A-I013 Text : 4 : PFOSA L34910-6 Spk D, 5000 n_L, DF=I0 073103A-1013 Sm (Mn, 2x3) 10C 01-Aug-2003 13:45:17 LC/MS/MS #E MRM of 4 ChannelsES- 9.88 498 > 78 65330- 3.48e5 Area (_ .... I ", r' , , _ .... 2.00 _ .... I .... 4.00 I' ' ' '' | .... 6.00 I .... I, , I '1 I ...... '"' '_ .... ,Time 8.00 10.00 12.00 F_ygen Research, 3058 Research Drive, State Colle_e, PA 16801 Quantify Sample Report _ Study No. zL34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 27 Decatur BC BC 080103 Name: 073103A-I014 Text : i: C8 Acid (PFOA) L34910-12 Spk E,5000 ng/L,DF=10 073103A-1014 Sm (Mn, 2x3) 1 iC,/= 01-Aug-2003 14:07:0_ LC/MS/MS #6 MRM of 4 ChannelsES- 4186519.14 2.49e6 i Area 413 > 369 (3 .... _-' ' ' ' _ .... 2.00 _ .... I .... 4.00 2:C6 Sulfonate (gFHS) L34910-12Spk E, 5000 ng/L, DF=10 073103A-1014 Sm (Mn, 2x3) 1 _ .... _ .... 6.00 _ .... _ ....... 8.00 . 5545 i .... 10.00 _ .... 1Time 12.00 01-Aug-200314:07:0 LC/MS/MS #6 MRM of 4 ChannelsES- 3.30e5 Area .... J .... c .... , .... , .... 2.00 4.00 3" C8 Sulfonate (PFOS) L34910-12Spk E, 5000 ng/i, DF-10 073103A-1014 Sm (Mn, 2x3) , .... , .... 6.00 _ .... , .... 8.00 M, . . . , .... 10.00 , .... ,Time 12.00 01-Aug-200314:07:06 LC/MS/MS#6 MRM of 4 ChannelsES- 9.24 499 > 99 Area 0 .... _,,, ,_ .... , .... _ .... _ ,",, ,I .... _.... _ .... _ .... _ .... _ .... 1Time V 2.00 4.00 6.00 8.00 10.00 12.00 Faygen Research, 3058 Research Drive, State College, PA 16801 Quantify San_le Study No.:L34910, Report Set No.:073103A, Ext.Date:07/31/03, _a_st:K.Ris_ Sample List: Last modifiedz Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslymx\Fluorochemlcals.PRO\Sam_leDB\O73103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Su_ Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 28 Decatur BC BC 080103 Name : 073103A-I014 Text : 4 : PFOSA L34910-12 Spk E, 5000 rig/L, DF=10 073103A-1014 10 Sm (Mn, 2x3) 01-Aug-2003 14:07:06 LC/MS/MS #6 MRM of 4 Channels ES- 9655 5.02e5 Area '' '', .... , .... 2.00 J .... , .... 4.00 , .... _ .... 6.00 , .... , .... 8.00 1 .... i .... 10.00 , .... 1Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _mf Study No.:L34910, Set No.:073103A, Ext.Dats:07/31/03, Analyst:x.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCM_MS6\Massllrnx\Fluorochemicals.PRO\MethDB\Deoatur Sun Aug 03 07:11:59 2003 Printed: Sun I Aug 03 07:19:29 2003 Page 29 Decatur BC BC 080103 Name: 073103A-I015 Text : i: C8 Acid (PFOA) !L34910-I6 Spk F,5000 ng/L,DF=I0 073103A-1015 Sm (Mn, 2x3) . 01-Aug-2003 14:28:57 LC/MS/MS #6 MRM of 4 ChannelsES- 9.13 413 > 369 1_i/1 0 I .... /".... , .... 2.00 _ .... i .... 4.00 2:C6 Sulfonate (PFHS) L34910-16 Spk F, 5000 ng/L, DF=I 0 073103A-1015 Sm (Mn, 2x3) 111 0 _.... ,, ,",,, .... , .... , .... 2.00 4.00 3:C8 Sulfonate (PFOS) L34910-16 Spk F, 5000 ng/i, DF=I 0 073103A-1015 Sm (Mn, 2x3) , .... , .... 6.00 , .... , .... 6.00 515606- 2.96e6Area ii t .... , ....... , .... ,...', i Time 8.00 10.00 12.00 01-Aug-2003 14:28:57 LC/MS/MS#6 MRM of 4 ChannelsES- 8.98 399 > 8(3 041 xe _ .... , .... , .... , .... , .... _Time 8.00 10.00 12.00 01 -Aug-2003 14:28:5"_ LC/MS/MS #e MRM of 4 ChannelsES- 9.25 499 > 99 Are, ,. 1(i/1 0-' .... , .... , .... 2.00 _ .... , .... 4.00 , .... , .... 6.00 1206971 , .... , .... , .... , .... 8.00 10.00 6.80e5 _ .... ,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:073103A, Ext.Date=07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:kDatakLCMS_6\Masslynx\Fluorocheunicals.PRO\MethDBkDecatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 30 Decatur BC BC 080103 Name: 073103A-I015 Text : 4 : PFOSA L34910-16 Spk F, 5000 ng/L, DF=I 0 073103A-1015Sm (Mn, 2x3) 10C % 01-Aug-2003 14:28:5 LC/MS/MS #_ MRM of 4 ChannelsES- 9.90 498 > 78 107094- 5.50e5 Area i C .... _' ," ,'"', .... 2.00 , .... ,,',, 4.00 ', .... , .... 6.00 ,'''" L"'""", 8.00 ....... 10.00 , .... _Time 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %_ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst=K.R/sha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073105A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslymx\Fluorohemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 31 Decatur BC BC 080103 Name: 073103A-I016 Text : i: C8 Acid (PFOA) XC072503-I, 25 n_L Standard 073103A-1016 Sm (Mn, 2x3) 01-Aug-2003 14:50:44 LC/MS/MS #6 MRM of 4 ChannelsES- 9.13 413 > 369 110/!v_, ,_,-_-_,/,/_,, , ,,,, , . , , ; , i _ _ , _ ,_ , , , ,"_6,9-,31..-._.. ", , , ...... 4f '38eT4iii i 2.00 4.00 6.00 8.00 10.00 12.00 %_ 2:C6 Sulfonate (PFHS) XC072503-1, 25 ng/L Standard 073103A-1016Sm (Mn, 2x3) 01-Aug-2003 14:50:44 LC/MS/MS #6 MRM of 4 ChannelsES- i/1 __ 100 ,t---_-/, ,_---:--_-7/, .... 2.00 ; , , _. 4.00 3:C8 Sulfonate (PFOS) XC072503-1, 25 ng/L Standard 073103A-1016 Sm (Mn, 2x3) , .... 6.00 8.9_ _-,. ; _; 1._.........._..8..96e3Area 8.00 10.00 399 > 80 Time 12.00 01-Aug-2003 14:50:44 LC/MS/MS #6 MRM of 4 ChannelsES- 9.26 499 > 99 11o/_, . 954-__5.75e3Area 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Reseuch, 3058 Research Drive, State College, PA 16801 Quantify Saz_le Report V Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\Saz_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 32 Decatur BC BC 080103 Name: 073103A-I016 Text : 4 : PFOSA XC072503-I, 25 n_L Standard 073103A-1016 Sm (Mn, 2x3) 01-Aug-2003 14:50:44 LC/MS/MS #6 MRM of 4 ChannelsES- 9.90 498 > 78 10C% 35451 1.95e4Area i C .... , .... , ,, , , , , ,",,., , , -,_ .... , .-, , , _ , , , ,-"T .... L .--r'. ,=',, , . ,Time 2.00 4.00 6.00 8.00 10.00 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemioals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 33 Decatur BC BC 080103 Name: Text: 073103A-I017 i: C8 Acid (PFOA) 534910-I 073103A-1017 Sm (Mn,2x3) 10C 01-Aug-2003 15:12:28 LC/MS/MS #6 MRM of 4 ChannelsES- 9.14 849301- 413 > 369 5.12e6 ! Area L C .... ' .... ] .... 2.00 I .... f .... 4.00 |* '', .... 6.00 , .... , .... 8.00 l''_ .... 10.00 , .... ,Time 12.00 %_ 2:C6 Sulfonate (PFHS) L34910-1 073103A-1017 Sm (Mn, 2x3) % 01-Aug-2003 15:12:28 LC/MS/MS #6 MRM of 4 ChannelsES- 8.99 399 > 80 Area 10C C i,, ,, , .... , .... 2.00 3:C8 Sulfonate 534910-1 (PFOS) , .... , .... 4.00 073103A-1017 Sm (Mn, 2x3) r .... + .... 6.00 501621 , .... ,., _, , .... ,,-, ,., 8.00 10.00 3.04e5 .,.. ,Time 12.00 01-Aug-2003 15:12:28 LC/MS/MS #_ MRM of4 ChannelsES- 9,25 499 > 99 Area 0 I .... , .... 'l .... 2.00 i .... i .... 4.00 u .... i .... 6.00 i .... _ .... 8.00 , .... I .... 10.00 , .... ,Time 12.00 E_ygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _i_ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified_ Methodl Last modified_ Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 34 Decatur BC BC 080105 Name: 075103A-I017 Text : 4 : PFOSA L34910-1 073103A-1017Sm(Mn,2x3) ..... 01-Aug-2003 15:12:28 LC/MS/MS #6 MRMof4 ChannelsES- 148109- 7.51 e5 Area 0 _''''' _.... , ' '" ' , .... _.... , .... , .... , .... _ .... , ....... 2.00 4.00 6.00 8.00 10.00 , .... ,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report q_ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 35 Decatur BC BC 080103 Name: Text: 073103A-I018 i: C8 Acid (PFOA) L34910-1 Rep 073103A-1018 Sm (Mn, 2x3) 01-Aug-2003 15:34:18 LC/MS/MS#6 MRM of 4 ChannelsES- 9.13 413 > 369 0 _ .... , .... , .... 2.00 , .... , .... 4.00 , .... , .... 6.00 i .... , ....... 8.00 %_ 2:C6 Sulfonate 534910-1 Rep (PFHS} 073103A-1018 Sm (Mn, 2x3) 9.00 ', .... 10.00 , .... ,Time 12.00 01-Aug-2003 15:34:1 LC/MS/MS #6 MRM of 4 ChannelsES399 > 80 % 10C C _.... , .... _ .... 2.00 3:C8 Sulfonate 534910-1 Rep (PFOS) , .... h .... 4.00 073103A-1018Sm (Mn, 2x3) , .... , .... 6.00 493421 , .... i .... , .... , .... 8.00 10.00 2.99e5Area , .... ,Time 12.00 01-Aug-2003 15:34:1 LC/MS/MS #_ MRM of4 ChannelsES- 9.26 499 > 99 Area 1(1 0' .... , .... , .... 2.00 ,.'... _ .... 4.00 i .... i .... 6.00 2741701 _ .... _ .... _ .... _ .... 8.00 10.00 1.56e6 _ .... _Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No. z073103A, Ext.Dats:07/31/03, Analyst:K.Risha San_le List= Last modifisdz Method: Last modified: Job Code: P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07=11=59 2003 Printed= Sun Aug 03 07:19z29 2003 Page 36 Decatur BC BC 080103 Name: 073103A-I018 Text : d : PFOSA L34910-1 Rep 073103A-1018 Srn (Mn, 2x3) ot10(_ ' '" ' _ .... , ,'_ , , , .... _ .... 2.00 4.00 i .... _ .... 6.00 01-Aug-2003 15:34:1 LC/MS/MS #6 MRM of 4 ChannelsES- 9.90 498 > 78 143575- 7.30e5 Area , .... , .... 8.00 L , ....... 10.00 , , , ,-_-_Time 12.00 V Exy_en Research, 3058 Research Drive, Stats College, PA 16801 I I I III Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemioals.PRO\MethDB\Decatur Sun Au_ 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 37 Decatur BC BC 080103 Name: 073103A-I019 Text : i: C8 Acid (PFOA) L34910-4 073103A-1019 Sm (Mn, 2x3) 01-Aug-2003 15:56:09_ LC/MS/MS #6 I MRM of 4 Channels ES- I 9.14 413 > 369I 1'o/1 575640- k 3.34e6Area l 0' .... _ .... j .... , .... 'l..'.., .... , .... , .... , ....... , .... _ .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 2:C6 Sulfonate L34910-4 (PFHS) 073103A-1019 Sm (Mn, 2x3) 01 -Aug-2003 15:56:09 LC/MS/MS #6 MRM of 4 ChannelsES- 8.98 399 > 80 3:C8 Sulfonate L34910-4 2.00 (PFOS) 073103A-1019 Sm (Mn, 2x3) ll0_ 4.00 0 '1.... , .... , .... , .... , ...., V 2.00 4.00 6.00 8.00 10.00 12.00 .... ,, .".., 6.00 01-Aug-2003 15:56:0 c LC/MS/MS #6 MRM of 4 ChannelsES- 9.26 499 > 99 211725-_ .... , .... 8.00 ii .... , .... 10.00 1.19e6 Area , .... ,Time 12.00 Exy_en Research, 3058 Research Drive, State College, PA 16801 Quantify Sample ReDort Study No.:L34910, Set No.:073103A, F_t.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Su_ Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 38 Decatur BC BC 080105 Name: 073103A-I019 Text : 4 : PFOSA L34910-4 .... 073103A-1019 Sm (Mn, 2x3) 10G 01-Aug-2003 15:56:09 LC/MS/MS #6 MRM of 4 ChannelsES- 9.91 498 > 78 106161- 5.46e5 Area ,i C .... I .... i .... 2.00 _ .... , .... 4.00 i .... I'''' 6.00 ,L J''' "' I .... i ....... 8.00 10.00 4 .... f Time 12.00 V FJcygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _df Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method= Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P=\Data\LCMSMS6\Massly_x\Fluorochemlcals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 39 Decatur BC BC 080103 Name: Text: 073103A-I020 i: C8 Acid L34910-2 (PFOA) 073103A-1020 Sm (Mn, 2x3) 01-Aug-2003 16:17:55 LC/MS/MS #6 MRM of 4 ChannelsES- 9.13 413 > 369 11=/1 605630J-L 3.4A9rea6 _: 0 _ .... , "" ' ' i .... , . . . . = .... _ . . '..'_... , , .... '_ .... _ , ,'_ .... _ .... ',Time 2.00 4.00 6.00 8.00 10.00 12.00 %1_ 2:C6 Sulfonate L34910-2 (PFHS) 073103A-1020 Sm (Mn, 2x3) 01-Aug-2003 16:17:5... LC/MS/MS #6 MRM of 4 ChannelsES- 8.98 399 > 80 100o0"_' r ' '' J .... : C8 Sulfonate L34910-2 _'' '1'', 2.00 (PFOS) .... , .... 4.00 073103A-1020 Sm (Mn, 2x3) , .... , .... 6.00 , .... , 3.6.22.'.31, .... _ .... 8.00 10.00 , .... ,2T.i1mAerea8e5 12.00 01-Aug-2003 16:17:55 LC/MS/MS #6 MRM of 4 ChannelsES- 9.27 499 > 99 Area ! 11o/1 1916311 1.08e6 0' .... , .... , .... .,...., .... ,...., .... ,..,., .... , .... , .... i .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Im_ Study No.:L34910, Set No.=073103A, Ext.Date:07/31/03, Analyst:K.Risha San_le List: Last modified: Method: Last modified: Job Code: Pz\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\San_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11z59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 40 Decatur BC BC 080103 Name: 073103A-I020 Text : 4 : PFOSA L34910-2 073103A-1020 Sm (Mn, 2x3) 01-Aug-2003 16:17:5_ LC/MS/MS #6 I MRM of 4 Channels ES- I 9,92 498 > 78I 11o/1 2.00 4.00 6.00 8.00 903641_0.00 12_4.0T.60Aim7reea5 _ 0 I ' ' ' } I '1 I '' , .... } .... _ .... , .... _ .... , .... , .... I .... ' .... _ .... V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify sample Study No.:L34910, Report Set No.:073103A, Ext.Date:07131/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LC_SMS6\Masslynx\Fluorochemicals.PRO\SamPleDB\073103A Sun Aug 03 07:08:13 2003 P:\DatakLCMSMS6\Masslynx\Fluorochemlcals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 41 Decatur BC BC 080103 Name: 073103A-I021 Text : i: C8 Acid (PFOA) L34910-3, DF=100 073103A-1021Sm (Mn, 2x3) 1 0o(_ 295299.13 01-Aug-2003 16:39:42 LC/MS/MS #6 MRM of4 ChannelsES- 1.73e5 413 > 369 i-_ .... _ , , , i .... i .... r, ,',', i .... i ,', , , , , , , ;i , , ,_.... , T, ', ",, J, _,, iTiAmreea i 2.00 4,00 6.00 8.00 10.00 12.00 2:C6 Sulfonate (PFHS) L34910-3, DF=100 073103A-1021Sm (Mn, 2x3) 01-Au g-2003 16:39:42 LC/MS/MS #6 MRM of 4 ChannelsES- 8,98 399 80 Area 1'i/1 0' .... , .... , . --._ , .... , .... 2.00 4.00 3:C8 Sulfonate (PFOS) L34910-3,DF=100 073103A-1021 Sm (Mn,2x3) , . . _ . , .... 6.00 4261 , .... , .... , .... , , .'.. 8.00 10.00 3.25e4 , .... ,Time 12.00 01-Aug-2003 16:39:42 LC/MS/MS #6 MRM of4 ChannelsES- 9.25 499 99 Area . 10o0-1 '/i-_,,,, V .... ,,-,. :, ...., .... 2.00 4.00 , .... , .... 6.00 60161 3.45e4 , .... , .... , .... , . ., ,.'.,_ ,Time 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No. z073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SamplsDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07_ii:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 42 Decatur BC BC 080103 Name: 073103A-I021 Text : 4 : PFOSA L34910-3, DF=100 073103A-1021 Sm (Mn, 2x3) 10(3 % 01-Aug-2003 16:39:42 LC/MS/MS #6 MRM of 4 ChannelsES- 9.92 - 498 > 78 9716- 5.15e4 Area i C _ .., _,'... _, ,,', _ .... ,', ,, . , .... _,', ,'., .... _, .'.. . ...... 2.00 4.00 6.00 8.00 10.00 ,'", _',. ,Time 12.00 %.S V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslymx\Fluorochemicals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07=ii:59 2003 Printed: S_n Aug 03 07:19:29 2003 Page 43 Decatur BC BC 080103 Name: 073103A-I022 Text : i: C8 Acid (PFOA) XC072503-2, 50 ng/L Standard 073103A-1022 Sm (Mn, 2x3) 01-Aug-2003 17:01:26 LC/MS/MS #6 MRM of 4 ChannelsES- 9.13 413 > 369 lq00/'1';'-_-,..._... _ , , ', j .... , .... ", .... , , , ,'. ,", . . , _ 1,3,78_0-1, .... j .... _ _; , ,-,8T.i4Am0rea4 ,11; 2.00 4.00 6.00 8.00 10.00 12.00 _I_ 2:C6 Sulfonate (PFHS) XC072503-2, 50 ng/L Standard 073103A-1022 Sm (Mn, 2x3) 01-Aug-2003 17:01:2E LC/MS/MS #6 MRM of 4 ChannelsES- 8.99 399 > 80 1i0_ ........ , .... 2.00 , .... , .... 4.00 3:C8 Sulfonate (PFOS) XC072503-2, 50 ng/L Standard 073103A-1022Sm (Mn, 2x3) , .... , .... 6.00 24201 ,.... , . ' , 8.00 9.24 , ,.... 10.00 1.50e4Area , .... ,Time 12.00 01-Aug-2003 17:01:26 LC/MS/MS #6 MRM of 4 ChannelsES499 > 99 ldl/lA - 0 r 1_ , :''' ' , .... 2.00 V , ' [ ' ' , .... , .... 4.00 6.00 16561 ' ' r , .... , .... ,,,, _ 8.00 10.00 9.73e3Area Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set NO.=073103A, Ext.Date:07/31/03, Analyst=K.Risha Sample List= Last modified: Method: Last modified: Job Code: P:\Data\LC_ISMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslyux\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page _4 Decatur BC BC 080103 Name: Text: 073103A-I022 4: PFOSA XC072503-2, 50 ng/L Standard 073103A-1022 Sm(Mn, 2x3) 01-Aug-2003 17:01:26 LC/MS/MS #6 MRMof4 ChannelsES- 9.89 498 > 78 111Ol 6634- _ 3.55e4Area li 0' i.... _ .... ,.... ,.... , _ , ,T, .... _.... ,_ _ .... _.... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 Ex3_en Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %_/ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Maeslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Paoe &5 Decatur BC BC 080103 Name: 073103A-I023 Text : i: C8 Acid L34910-6 {PFOA) 073103A-1023 Sm (Mn,2x3) ' 01 -Aug-2003 17:23:17 LC/MS/MS #6 MRM of 4 ChannelsES- 173871 1.01e6 Area i YIl . , ,_--_..,, .... 2.00 , .... i .... 4.00 , .... , .... 6.00 , .... , .... 8.00 , .... , .... 10.00 , .... ,Time 12.00 _ 2:C6 Sulfonate (PFHS) 534910-6 073103A-1023 Sm (Mn, 2x3) 01-Aug-2003 17:23:17 LC/MS/MS #6 MRM of 4 ChannelsES- 8.99 399 > 80 llo/l 0'....-1 .... i .'... r .... , .... 2.00 4.00 3:C8 Sulfonate 534910-6 (PFOS} 073103A-1023 Sm (Mn, 2x3) , .... , .... 6.00 / 86861 5.16e4Area , .... J .... i ' ' ' _, ' '"' ' , .... ,Time 8.00 10.00 12.00 01-Aug-2003 17:23:17 LC/MS/MS #6 MRM of 4 ChannelsES- 9.25 499 > 99 Area 1i0-_ YlI .... j .... , .... 2.00 , .... ,.,,., 4.00 .... , .... 6.00 449221 _ .... _ .... , .... , .... 8.00 10.00 2.66e5 ,...', ,Time 12.00 Ex_gen Research, 3058 Research Drive, State College, PA 16801 Q_antify Sample Report _ Study No.=L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page &6 Decatur BC BC 080103 Name: 073103A-I023 Text : 4 : PFOSA L34910-6 073103A-1023 Sm (Mn, 2x3) 01-Aug-2003 17:23:17 LC/MS/MS #6 MRM of 4 ChannelsES- 9.88 498 > 78 l(a_ .. 19717-i L 1.01e5Area i 0 I .... I .... _ , r'=', , ] .... _ .... I .... J .... , .... I .... I .... ") )' I .... _Time 2.00 4.00 6.00 8,00 10,00 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study Mo.:L34910, Report Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 47 Decatur BC BC 080103 Name: 073103A-I024 Text : I: C8 Acid (PFOA) L34910-6 Rep 073103A-1024Sm (Mn, 2x3) 01 -Aug-2003 17:45:07 LC/MS/MS #6 MRM of 4 ChannelsES- 9.13 413 > 369 11'o O' .... _--' ' ' I .... 2.00 i .... _ .... 'r', , , . _ .... 4.00 6.00 [, , , , I .... 8.00 ' . , , _ .... 10.00 ,oa _ .". , , _Time 12.00 %_ 2:C6 Sulfonate (PFHS) L34910-6 Rep 073103A-1024 Sm (Mn, 2x3) 01-Aug-2003 17:45:07 LC/MS/MS #6 MRM of4 ChannelsES- 8.97 399 > 80 1ql0 _ .... _ , r.. , .... 2.00 _ .... , .... 4.00 3:C8 Sulfonate L34910-6 Rep (PFOS) 073103A-1024Sm (Mn, 2x3) , .... i .... 6.00 i .... , ..8..505_, . .o.. , _, . . , .... ,5T.i2m3ee4Area 8.00 10.00 12.00 01-Aug-2003 17:45:07 LC/MS/MS #6 MRM of 4 ChannelsES- 9.25 499 > 99 Area 0',,',, I .... , .... ,,-,.,, .... , .... , .... , .... ",',,,. _ .... , .... , .... ,Time V 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.=L3_910, Report Set No.:073103A, Ext.Date=07/31/03, Analyst=K.Risha Sample List= Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\San_leDB\073103A Sun Aug 03 07=08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed= Sun Aug 03 07:19:29 2003 Page 48 Decatur BC BC 080103 Name: 073103A-I024 Text : 4 : PFOSA L34910-6 Rep 073103A-1024 Sm (Mn, 2x3) 01-Aug-2003 17:45:07j LC/MS/MS #6 I MRM of 4 Channels ES- t 9.90_ 498>78 I 11/I 20175 L 1.01e5Area _ 0 _ .... J .... , .... , .... , .... , .... , .... , .... , .... r .... _ .., .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 I I I _a_tify Sample Report %_ Study No.:L3_910, Set No.:073103A, Ext.D_te=07/31/03, _aly_t:K.Risha Sample List= Last modified= Method: Last modified: Job Code: P:kData\LCMSMS6\Massly_x\Fluorochemicals.PRO\SampleDBk073103A Sun Aug 03 07:08=13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed= Sun Aug 03 07:19:29 2003 Page 49 Decatur BC BC 080103 Name: 073103A-1025 Text : 1:C8 Acid L34910-9 (PFOA) 073103A:1025Sm (Mn, 2x3) 1I_ 01-Aug-2003 18:06:53 LC/MS/MS #6 9.13 355190- MRM of 4 ChannelsES413 > 369 2.13e6 . Are_ i 1 0 I .... , ,-..., .... 2.00 ,,. ,,,, ,-,,, .... , .... 4.00 6.00 _ .... _ ....... 8.00 k "_'"',, ' r .... ,Time 10.00 12.00 %_ 2:C6 Sulfonate (PFHS) !L34910-9 073103A-1025Sm (Mn, 2x3) 10 2109 01-Aug-2003 18:06:53 LC/MS/MS #6 MRM of4 ChannelsES- 1.26e5 Area 0 ' .... "J .... } '--' 2.00 " I _ .... 3:C8 Sulfonate 'L34910-9 (PFOS) 073103A-1025 Sm (Mn, 2x3) ] .... 4.00 ] .... J .... 6.00 J .... J .... 8.00 J .... , .... 10.00 J .... ,Time 12.00 01-Aug-2003 18:06:53 LC/MS/MS #6 MRM of4 ChannelsES- 9.24 499 > 99 10=01 i I .... _ .... _,.,.., 2.00 .... ,.... 4.00 ,.... ,.... 6.00 112926_ ,.... ,..'.',, .... , .... 8.00 10.00 6.60eSArea j .... ,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\DatakLCMSMS6kMasmlynx\Fluorochemicals.PRO\MethDB\Decatur Su_ Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 50 Decatur BC BC 080103 Name: 073103A-I025 Text : 4 : PFOSA L34910-9" "" 073103A-1025 Sm (Mn, 2x3) 01-Aug-2003 18:06:53 LC/MS/MS #6 MRM of 4 ChannelsES- 9.88 498 > 78 i1110_ 523631 2.66e5Area i: ' ' ' _" '' ' I .... , .... _ .... _ .... _ .... , ' ' "' , .... , .... i .... J .... _Time 2.00 4.00 6.00 8.00 10.00 12.00 Exyven Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08=13 2003 P;\Data\LCMSMS6kMasslynx\Fluorocheunicals.PROkKethDB\Decatur Sun Aug 03 07;ii:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 51 Decatur BC BC 080103 Name: 073103A-I026 Text : i: C8 Acid L34910-7 (PFOA) 073103A-1026 Sm (Mn, 2x3) 01-Aug-2003 18:28:44 LC/MS/MS #6 MRM of 4 ChannelsES- 9.13 413 > 369 10<:o 52136a 2.97e6Area t C .... _ .... , .... I .... _ .... I .... , '' ' ", .... , ''' ' i .... , .... , .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 2:C6 Sulfonate L34910-7 (PFHS} 073103A-1026 Sm (Mn, 2x3) 01-Augo2003 18:28:44 LC/MS/MS #6 MRM of 4 ChannelsES- 8.98 399 > 80 1i1 ."...,.... ,.... ,'....,....', .... , .... , .'.',.,3.3.9.6.51 ,.... ,.... , .... 2,.T0i4mee5Area 2.00 4.00 6.00 8.00 10.00 12.00 3:C8 Sulfonate L34910-7 (PFOS) 073103A-1026 Sm (Mn, 2x3) 01-Aug-2003 18:28:44 LC/MS/MS #6 MRM of 4 ChannelsES- 9.26 499 > 99 11o/l 0 I .... J .... ,.'. ,-., .... ",,.', .', .... ,, ..,,. 2.00 4.00 6.00 1490881 ,,., .... , .... , .... 8.00 10.00 8.38e5Area i .... ,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 I III I Quantify Sample Study No.:L34910, Report Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Massly_x\Fluoroche3_icals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: S_ul Aug 03 07:19:29 2003 Page 52 Decatur BC BC 080103 Name. 073103A-I026 Text : 4 : PFOSA L34910-7 073103A-1026Sm (Mn, 2x3) 01-Aug-2003 18:28:44 LC/MS/MS #E MRM of 4 ChannelsES- 9.92 498 > 78 10o0_ 67031_ 3.A44rea5 t:' .... _.,,.., .... ,.,.. ,, .... , .... , .... , .... ,-,.,., ,-,,., , .... _ .... _Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Page 53 Sample Lint: Last m_dified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals. PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochem/cals.PRO\MethDBkDecatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Sun Aug 03 07:19:29 2003 Name: 073103A-I027 Text : : C8 Acid (PFOA) L34910-8, DF=100 073103A-1027 Sm (Mn, 2x3) ' 01-Aug-2003 18:50:3(] LC/MS/MS #6 MRM of 4 ChannelsES- 9.13 413 > 369 Area 11o/1 0_--_,,, ,-_-, ; ......,.............,.... , ,j , , , , 2.00 4.00 6,00 t_ 2:C6 Sulfonate (PFHS} L34910-8, DF=100 073103A-1027 Sm (Mn, 2x3) 215961 ,-- ....... _ 8.00 ., T,., 10.00 1.32e5 , , -, _Time 12,00 01-Aug-2003 18:50:3(] LC/MS/MS#6 MRM of 4 ChannelsES- 8.97 399 > 80 11o/! 0 I .... , .... C.... 2.00 3:C8 Sulfonate (PFOS) L34910-8, DF=100 _ .... i .... 4.00 073103A-1027 Sm (Mn, 2x3) 53421 3.1Area0e4 _'' '_ ' _''" ''t .... ,", , , _ .... "_,.', ,',,, ._ ,Time 6.00 8.00 10.00 12.00 01-Aug-2003 18:50:3(] LC/MS/MS #6 MRM of 4 ChannelsES- 9.25 499 > 99 1(o0/, _ , ' , , , , ,-, ,, , ,, 2.00 , , , , , m,, , , ,, 4.00 iI , , , , , , , , , _-, , , , , , , 4, 3, 33,1, , , , ," , 6.00 8.00 10.00 , ,"_ , , , , ,2T.i6m7ee4Area 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.=L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha San_le List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 54 Decatur BC _C 080103 Name: 073103A-I027 Text : 4 : PFOSA L34910-8, DF=100 073103A-1027Sm (Mn, 2x3) 110 _ '' i .... J .... 2.00 "i .... 'i'' 4.00 " ' i .... l "_' '6.00 i .... , .... 8.00 01-Aug-2003 18:50:3C LC/MS/MS #6 MRM of 4 ChannelsES- 9.90 498 78 5639- Area 3.03e4 iL _'_ ...... 0.00 ,"''' iTime 12.00 ql_Bl' Ex1_en Research, 3058 Research Drive, State College, pA 16801 Quantify Sample Report q_ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluoroahemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 55 Decatur BC BC 080103 Name: 073103A-I028 Text : i: C8 Acid (PFOA) _XC072503-3, 100 ng/L Standard 073103A-1028 Sm (Mn, 2x3) 01-Aug-2003 19:12:20 MRM of 4LCCh/MaSnn/MeSlsES#6- 9.15 413 > 369 0'=., . i .-7".'.,'.'i.'.'.._. , ' l ' ,",, J .... I .... I .... i ' ' ' ' _ , ' _ ' _ .... "i '" L,_,I .... i Time 2.00 4.00 6.00 8.00 10.00 12.00 _ 2:C6 Sulfonate (gFHS) XC072503-3, 100 ng/L Standard 073103A-1028 Sm (Mn, 2x3) 01-Aug-2003 19:12:20 LC/MS/MS #6 MRM of 4 ChannelsES- 8.98 399 > 80 1_i/1 OLd, , , _=--,- i j .... 2.00 i ' '=' r'l _"' ' ' r .... 4.00 J .... 6.00 3:C8 Sulfonate (PFOS) XC072503-3, 100 ng/L Standard 073103A-1028 Sm (Mn, 2x3) 5959-_ 3.59e4Area a , " J , , , , i c , , , _ . , ,_, J .... ,Time 8.00 10.00 12.00 01-Aug-2003 19:12:2( LC/MS/MS #E MRM of 4 ChannelsES- 9.27 499 99 1_i/1 0J I;'' r' '', ?' '' '_ ''' 2.00 ' i 1 .... I , ' '- I , .... 4.00 , .... 6.00 35001 2.09e4Area , .... , .... , .... -,-=", , , , .... -, Time 8.00 10.00 12.00 F..xygen Reseuch, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method= Last modified: Job Code: P:\Data\LCMSMS6\Masslln_x\Fluorochamlcals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemioals.PRO\MethDB\Decatur Su_ Aug 03 07:11:59 2003 Prin_ed: Sun Aug 03 07=19:29 2003 Page 56 Decatur BC BC 080103 Name: 073103A-I028 Text : 4 : PFOSA XC072503-3, 100 ng/L Standard 073103A-1028 Sm (Mn, 2x3) ot100-_ '/o 01-Aug-2003 19:12:2C LC/MS/MS #6 MRM of 4 ChannelsES- 9.90 498 > 78 13989" 7.45e4 Area _ .... _ .... _ .... _ .... _ .... _ .... _ .... _ .... _ .... _ ....... 2.00 4.00 6.00 8.00 10.00 _. ,",. _Time 12.00 V E_Ygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %_J Study No.:L34910, Set No.=073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 57 Decatur BC BC 080103 Name : 073103A-I029 Text : i: C8 Acid (PFOA) IL34910-I2 073103A-1029Sm (Mn, 2x3) 01-Aug-2003 19:34:0." LC/MS/MS #6 MRM of4 ChannelsES- 9.14 413 > 36S 1'11 2,71389- L 1.47e7Area 1 0 I'' ''' ,''' ', .... ,' ''', .... , .... r .... , .... , ....... , .... , .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 %_ 2:C6 Sulfonate (PFHS) L34910-12 073103A-1029 Sm (Mn, 2x3) 01-Aug-2003 19:34:0." LC/MS/MS #6 MRM of 4 ChannelsES- 8.99 399 > 8(] 1'i/l 0t.... , .... o .... 2.00 I .... , , . . . , .... , .... 4.00 6.00 3:C8 Sulfonate L34910-12 (PFOS} 073103A-1029 Sm (Mn, 2x3) 259042_ , .... , .... t .... ,..-.. 8.00 10.00 1.50e6Area , .... ,Time 12.00 01-Aug-2003 19:34:03 LC/MS/MS #6 MRM of 4 ChannelsES- 9.27 499 > 99 Ares %_lf i1 ' '" ' I .... I ' ' ' ' I .... 2.00 I ' ' ' ' I "' 4.00 , '""' '"' t"' ' ' " t . . .... ) 6.00 8.00 ' ' [ ' ' ' ' _ " ' ' ' , Time 10.00 12.00 Faygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:073103A, Ext.Date:07131/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\FlUorochemicals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslyr_\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 58 Decatur BC BC 080103 Name: Text: 073103A-I029 4: PFOSA L34910-12 073103A-1029Sm (Mn,2x3) 01-Aug-2003 19:34:02 LC/MS/MS #6 MRMof4 ChannelsES- 9.90 498 > 78 lci/1 1.36e6A, 1 0" .... _.... I "'' _.... i .... I .... L.... _ .... _.... _ ....... 2.00 4.00 6.00 8.00 10.00 _.... i_me 12.00 I,,.# Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:073103A, Ext.Date:07/31/03, Analyst:X.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Massly_xkFluorochemicals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 59 Decatur BC BC 080103 Name: 073103A-I030 Text : 1:C8 Acid (PFOA) L34910-12 Rep 073103A-1030Sm (Mn,2x3) i 1,__, i _'_ 9.11 2425189- 01-Aug-2003 19:55:50 LC/MS/MS #6 MRM of 4 ChannelsES413 > 369 Area 1.43e7 " ' ' ' , ' ' ' ' , .... 2.00 2:C6 Sulfonate L34910-12 Rep (PFHS) i .... , .... 4.00 073103A-1030 Sm (Mn, 2x3) , .... , .... 6.00 , .... I ....... 8.00 8.98 , .... 10.00 , .... ,Time 12.00 01-Aug-2003 19:55:50 LC/MS/MS #6 MRM of 4 ChannelsES399 > 80 Area 1i0_ 2376491 1.45e6 .... ,.... ,.... , .... L .... ,.... L.... , .... _.... , .... _.... ,.... _Time 2.00 4.00 6.00 8.00 10.00 12.00 3:C8 Sulfonate L34910-12 Rep (PFOS) 073103A-1030 Sm (Mn, 2x3) 01oAug-2003 19:55:50 LC/MS/MS #6 MRM of 4 ChannelsES- 9.24 499 > 99 Area 1i_ i1 .... ' .... ' .... 2.00 , .... J .... 4.00 , .... , .... 6.00 5712111 3.17e6 | .... , ,, ,, , ,, , ,,,, , ', .... ,Time 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %_ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analys_:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\Sam_leDB\073103A Sun Au R 03 07z08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur Su_ Aug 03 07:11:59 2003 Printed: Stuz Aug 03 07:19:29 2003 Page 60 Decatur BC BC 080103 Name: 073103A-I030 Text : 4 : PF6SA L34910-I2 Rep 073103A-1030 Sm (Mn, 2x3) 01-Aug-2003 19:55:5C LC/MS/MS#6 MRM of 4 ChannelsES- 9.90 498 > 78 1i0_. 2634111 1.A32rea6 1 .... ..-,., .... ,.... j .... , .... , .... _ .... , .... , ....... , .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 V ExyRen Research, 3058 Research Drive, State College, PA 16801 I II Quantify Sample Report _ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluoroche_icals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\MasslynxkFluorochemlcals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19=29 2003 Page 61 Decatur BC BC 080103 Name: 073103A-I031 Text : 1:C8 Acid L34910-15 (PFOA) 073103A-1031 Srn (Mn, 2x3) 01-Aug-2003 20:17:38 LC/MS/MS #6 MRM of 4 ChannelsES- 9.13 413 > 369 110_ 2527002- 1.47e7Area i .... , ,,. _ .... 2.00 tt_lf 2:C6 Sulfonate L34910-15 (PFHS) , .. ,.,.., 4.00 073103A-1031Sm (Mn, 2x3) .... , .... , .... , ....... 6.00 8.00 8.98 ,,,.., 10.00 .... ,Time 12.00 01-Aug-2003 20:17:38 LC/MS/MS #6 MRM of 4 ChannelsES399 > 80 110 _ 0 .... , .... , ,., . . , .... , .... 2.00 4.00 3:C8 Sulfona_e L34910-15 (PFOS) 073103A-1031 Sm (Mn, 2x3) i .... , .... 6.00 2456871 1.43e6Area , .... , .... i .... ,. , . . , .... ,Time 8.00 10.00 12.00 01-Au g-2003 20:17:3E LC/MS/MS #E MRM of 4 ChannelsES- 9.25 499 > 9_ _idB 11o/1 0 =.... ,.,,,, .... 2.00 _ .... = .... 4.00 ,.,.., .... 6.00 560118_ , .... ,..,,, .... , .... 8.00 10.00 3.15eEAre , .... ,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify San_le ReDort _ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, AnalystzK.Risha Sample List: Last modlfied: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19z29 2003 Page 62 Decatur BC BC 080103 Name; 073103A-I031 Text : 4 : PFOSA L34910-15 073103A-1031 Sm (Mn, 2x3) 01-Aug-2003 20:17:38 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 78 0 I, , ,, t , , , , _ .... 2.00 _ .... , .... 4.00 _ .... i .... '_ .... _ .... 6,00 8.00 , .... L .... 10.00 , .... i Time 12.00 V Exy_en Research, 3058 Research Drive, State College, PA 16801 Quantify sa=_le ReDort q',a_ Study No.:L34910, Set No.:073103A, Ext.Date:07131/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\MasslynxkFluorochemicals.PRD\Sam_leDBk073103A Sun Aug 03 07=08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 63 Decatur BC BC 080103 Name: 073103A-I032 Text : i: C8 Acid L34910-13 (PFOA) 073103A-1032Sm (Mn, 2x3) 10 284987 01-Aug-2003 20:39:25 LC/MS/MS #6 MRM of 4 ChannelsES- 1.69e7 Area 0 1.... _ . , . . _ .... 2.00 _ .... _ .... 4.00 L .... _ .... 6.00 _ .... , .... 8.00 _ .... , .... 10.00 , .... _Time 12.00 %_ 2:C6 Sulfonate L34910-13 (PFHS) 073103A-1032Sm (Mn, 2x3) 10 27585 01-Aug-2003 20:39:25 LC/MS/MS #6 MRM of 4 ChannelsES- 1.67e6 Area C _, , .', , .... , .... 2.00 3:C8 Sulfonate L34910-13 (_FOS_ ,.... t .... 4.00 073103A-1032 Sm (Mn, 2x3) , ...... , .... 6.00 , .... , .... 8.00 , .... , .... 10.00 , .... ,Time 12.00 01-Aug-2003 20:39:25 LC/MS/MS #6 MRM of 4 ChannelsES- 9.24 499 > 99 1(o/i 0" .... , .... , .... 2.00 , .... _ .... 4.00 _ .... , .... 6.00 6671861 , .... ", .... , .... , .... 8.00 10.00 3.69e6Area ,'.... ,Time 12.00 Exygen Research, 3058 ReJearch Drive, State College, PA 16801 Quantify Sample Report i_ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 64 Decatur BC BC 080103 Name- 073103A-I032 Text : 4 : PFOSA L34910-13 073103A-1032Sm (Mn,2x3) 01-Aug-2003 20:39:25 LC/MS/MS#6 MRMof4 ChannelsES- 9.90 498 > 78 1 1 0 I .... , .... , .... ; .... I .... I .... , .... , .... , .... _L , ....... ,. r.. ,Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quamtify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07131/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 65 Decatur BC BC 080103 Name: 073103A-I033 Text : i: C8 Acid (PFOA) L34910-14, DF=100 073103A-1033 1007 Sm (Mn, 2x3) 01-Aug-2003 21:00:58 LC/MS/MS #6 MRM of 4 Channels ES- 9.12 413 > 369 71294" 4.14e5 Area t 4 0 _' ' ' 'T_ .... ,'" ' _' J .... 2.00 ', .... 4.00 2:C6 Sulfonate (PFHS) L34910-14, DF=100 073103A-1033 Sm (Mn, 2x3) i .... _ .... 6.00 , .... , ....... 8.00 8:96 i ,'"'' 10.00 _ .... ,Time 12.00 01-Aug-2003 21:00:58 LC/MS/MS #6 MRM of 4 Channels ES399 80 111/l 0_, ,. ,",... i .... 2.00 , .... , .... 4.00 3:C8 Sulfonate (PFOS) L34910-14, DF=100 073103A-1033 Sm (Mn, 2x3) T.. ,',, .... 6.00 9718 1 , .... _ .... , .... , .... 8.00 10.00 5.83e4Area ,..,., ,Time 12.00 01-Aug-2003 21:00:58 LC/MS/MS #6 MRM of 4 Channels ES- 9.24 499 99 1_i/1 0_,,., ,'.,.,, .... 2.00 , .... , .... 4.00 , .... , .... 6.00 ', .... 14981_ , .... , .... 8.00 , .... 10.00 8.40e4Area _ .... _Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A S_u_ Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Au_ 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 66 Decatur BC BC 080103 Name: 073103A-I033 Text : 4 : PFOSA L34910-14, DF=100 073103A-1033Sm (Mn, 2x3) 1 i0_ 01-Aug-2003 21:00:58 LC/MS/MS #6 MRM of 4 ChannelsES- 11410- 9.90 5.88e4 Area ,. 498 > 78 1 .... , .... , .... , .... , .... '_ .... , .... , .".. , , .... _ .',, .... , .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:073103A, Ext.Date:07131/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sa_pleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 67 Decatur BC BC 080103 Name: 073103A-I034 Text : i: C8 Acid (PFOA) . XC072503-4, 250 ng/L Standard 073103A-1034 Sm (Mn, 2x3) 01-Aug-2003 21:22:34_ LC/MS/MS #6I MRM of 4 ChannelsES- I 9.13 413 > 369I 11/1 75537- k 4.32e5Area i 0' .... ,i-<_, _, , .... , .... , .... , .... , .... ,' '"' , ....... ,''' " I '' "' i Time 2.00 4.00 6.00 8.00 10.00 12.00 %_ 2:C6 Sulfonate (PFHS) XC072503-4, 250 ng/L Standard 073103A-1034 Sm (Mn, 2x3) 01-Aug-2003 21:22:34 LC/MS/MS #6 MRM of 4 ChannelsES- 8.98 399 > 80 OJ "" ' '', ' "', .... 2.00 , .... , .... 4.00 3:C8 SulfonaCe (PFOS) XC072503-4, 250 ng/L Standard 073103A-1034 Sm (Mn, 2x3) , .... r .... 6.00 , , ' ,........ , , .... 8.00 ,,, , 10.00 , , ,-,,Time 12.00 01-Aug-2003 21:22:34 LC/MS/MS #6 MRM of 4 ChannelsES- 9.25 499 > 99 11!0'_, , . , .... _ .... , , , ,', _ .... r,_ ,', _ , . ,L .... , .', 8, 5.2L1_..L.. ,, , , ,'_ ,',, , ,4T.i9m1ee4Area V 2.00 4.00 6.00 8.00 10.00 12.00 E_ygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No._L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha San_le List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\San_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 68 Decatur BC BC 080103 Name: 073103A-I034 Text : 4 : PFOSA XC072503-4, 250 ng/L Standard 073103A-1034Sm (Mn, 2x3) 10 01-Aug-2003 21:22:34 LC/MS/MS #6 MRM of 4 ChannelsES- 3386 1.75e5 Are_ 0 I .... _ .... , .... 2.00 ........ 4.00 _ .... _ .... 6.00 _ .... _ .... 8.00 _ .... _ .... 10.00 _ .... _Time 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.=073103A, Ext.Date:07/31103, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sa_pleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed= Sun Aug 03 07:19:29 2003 Page 69 Decatur BC BC 080103 Name= 073103A-I035 Text : i: C8 Acid L34910-16 (PFOA) 073103A-1035 Sm (Mn, 2x3) 10C . .01-Aug-2003 21:44:25 " LC/MS/MS #6 MRM of 4 ChannelsES- 9.11 413 > 369 3072978- 1.85e7 Area _ 2.00 _bulf 2:C6 Sulfonate L34910-16 (PFHS) 073103A-1035 Sm (Mn, 2x3) 10 4.00 6.00 8.00 28351 10.00 12.00 01-Aug-2003 21:44:25 LC/MS/MS #6 MRM of4 ChannelsES- 1.74e6 Area 0' .... , .... , .... 2.00 3:C8 Sulfonate L34910-16 (PFOS) , .... r .... 4.00 073103A-1035 Sm (Mn, 2x3) _ .... , .... 6.00 i .... ', .... 8.00 , .... , .... 10.00 , .... ,Time 12.00 9,24 69116 01-Aug-2003 21:44:25 LC/MS/MS #61 MRM of 4 ChannelsES499 > 99J 3.86e6 Area O' .... , .... , .... , .... , .... ', .... ', .... , .... , .... _ .... , .... , .... ,Time V 2.00 4.00 6.00 8.00 10.00 12.00 Exy_en Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Re_ort _ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, AnalystzK.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: - Sun Aug 03 07:19:29 2003 Page 70 Decatur BC _C 080103 Name: 073103A-I035 Text = 4 : PFOSA L34910-16 073103A-1035Sm (Mn, 2x3) 01-Aug-2003 21:44:25 LC/MS/MS #6 MRM of 4 ChannelsES- 9.90 498 > 78 1'o/1 358032-, , 1.82e6Area !: O' .... , .... ,,, ,",, ,",,,, .... , .... , .... , .... , .... , ....... , .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 71 Decatur BC BC 080103 Name: 073103A-I036 Text : i: C8 Acid (PFOA} L34910-16 Rep 073103A-1036 Srn (Mn, 2x3) 01-Aug-2003 22:06:04_ LC/MS/MS #6I MRM of 4 ChannelsES- I 9.13 413 > 369 1.89e7' .. Area 0' .... ''''' '2.00.... ' .... 4.00.'... ''''' '6.00.... ' .... 8.00.'... "'''I0.00 .... '' ' ' 11'2T'i.uImu e _ 2:C6 Sulfonate (PFHS) L34910-16 Rep 073103A-1036Srn (Mn, 2x3) 01-Aug-2003 22:06:04 LC/MS/MS #6 MRM of 4 ChannelsES- 8.98 399 > 80 Area 0 'i .... , .... , .... 2.00 3:C8 Sulfonate L34910-16 Rep _PFOS) , ..... L .... 4.00 073103A-1036 Sm (Mn, 2x3) ) .... _ .... 6.00 , .... , .... 8.00 ,,.. '. , .... 10.00 , .... )Time 12.00 01-Aug-2003 22:06:04 LC/MS/MS #E MRM of 4 ChannelsES-: 9.25 499 > 99 Area .... , .... , .... , .... , .... , .... , .... j .... , .... , .... , .... , .... ,Time V 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 72 Decatur BC BC 080103 Name: 073103A-I036 Text : 4 : PFOSA L34910-16 Rep 073103A-1036Sm (Mn, 2x3) 01-Aug-2003 22:06:04 LC/MS/MS #6 MRM of 4 ChannelsES- 9.90 498 > 78 110-_ 358872- i.83e6Area .... , .... I _ ' '' I .... , .... , .... J .... [ .... , .... i ....... 2.00 4.00 6.00 8.00 10.00 , .... i Time 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 I I Quantify Sample Report %_ Study No.:L34910, Set NO.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Me_hod: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\San_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Stul Aug 03 07:11:59 2003 Printed= Sun Aug 03 07:19:29 2003 Page 73 Decatur BC BC 080103 Name: 073103A-I037 Text : 1:C8 Acid L34910-19 {PFOA) 073103A-1037Sm (Mn, 2x3) i '" 01-Aug-2003 22:27:50 LC/MS/MS #6 MRM of 4 ChannelsES- 9.11 413 > 369 Area ; 1'i/1 2758295- I 1.68e7 ! 0'.. ' i .... , .... , .... ,'' ' ' , .... , .... , .... r' ...... ,..,. ,.... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 _ 2:C6 Sulfonate (PFHS) L34910-19 073103A-1037Sm (Mn, 2x3) 01-Aug-2003 22:27:50 LC/MS/MS #6 MRM of 4 ChannelsES- 8.98 399 > 80 111/1 0 I .... J .... ) .... 2.00 J .... , .... 4.00 3:C8 Sulfonate L34910-19 (PFOS) 073103A-1037 Sm (Mn, 2x3) 2764291 ? .... , ,... , , . . . . ) .... , .... , .... 6.00 8.00 10.00 1.67e6Area , . . . ,Time 12.00 01-Aug-2003 22:27:51_ LC/MS/MS #6I MRM of 4 ChannelsES- I 9.24 499 > 99} Area 1ti/I 0 { .... | .... | .... 2.00 I .... , '"'' 4.00 , .... , .... 6.00 6565331 , .... , .... , .... , .... 8.00 10.00 3.82e6; , .... ,Time 12.00 F..xygen Research, 3058 Research Drive, State College, PA 16801  M_ Quantify San_le Study No.:L34910, Report Set No.=073103A, Ext.Date=07/31/03, Analyst:K.Risha San_le List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicale.PRO\SampleDB\073103A Sun Aug 03 07=08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11=59 2003 Printed: Sun Aug 03 07=19=29 2003 Page 74 Decatur BC BC 080103 Name: Text: 073103A-I037 4: PFOSA L34910-19 073103A-1037 Sm (Mn, 2x3) 01-Aug-2003 22:27:50 LC/MS/MS #6 MRM of 4 ChannelsES- 9.87 498 > 78 111 369645_ 1.A89rea6 ' 0 '_.... , .... , .... , .... i .... , .... , .... , .... _ .... , .... = .... J .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %_ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Su_ Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MsthDB\Decatur Su_ Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 75 Decatur BC BC 080103 Name: 073103A-I038 Text : i: C8 Acid L34910-17 (9FOA) 073103A-1038 Sm (Mn, 2x3) 01-Aug-2003 22:49:4( LC/MS/MS#E MRM of 4 ChannelsES- 3102823" 1.85e7 Area _ Yo I 1 .... _ .... _' ""' _ .... i .... 2.00 4.00 _ .... i .... 6.00 _ .... _ ....... Ji, 8.00 i .... 10.00 i .... _Time 12.00 2:C6 Sulfonate L34910-17 (PFHS) )73103A-1038 Sm (Mn, 2x3) 10(3 % 0 .... , .... , .... 2.00 , .... , .... 4.00 _ .... , .... 6.00 ., . , 8.98 l278698-_ ., .... i .... 8.00 01-Au g-2003 22:49:4( LC/MS/MS #(3 MRM of 4 ChannelsES- i 399 > 80 1.69e6 Are_ , .... 10.00 , .... ,Time 12.00 3:C8 Sulfonate (9FOS) L34910-17 01-Aug-2003 22:49:4 LC/MS/MS #6 073103A-1038 Sm (Mn, 2x3) MRM of 4 ChannelsES- 9.24 499 > 99 10'..,'., .... ,.... , .... , .... _ .... _ .... j .... , .... , .... , .... ,.... ,Time V 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, S_ate College, PA 16801 Quantify Sample Report _,_ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modiied: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07=08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 76 Decatur BC BC 080103 Name: 073103A-I038 Text : 4 : PFOSA L34910-17 073103A-1038Sm (Mn, 2x3) 01-Aug-2003 22:49:40 LC/MS/MS #6 MRM of 4 ChannelsES- 9.90 498 > 78 lql/1 311246-j _ 1.60e6Area !: 0 I .... , .... , .... , .... , .... , .... , .... , .... , .... , ....... j .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List= Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Deoatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 77 Decatur BC BC 080103 Name: 073103A-I039 Text : i: C8 Acid (PFOA) L34910-18, DF=100 073103A-1039 Sm (Mn, 2x3) ." .01-Aug-2003 23:11:3_ LC/MS/MS #6 MRM of 4 Channels ES- 9.12 413 > 369 1(i/1 77205- L 4.47e5Area 1 0L_,, .. ,_ . :' w .... L' ' ' i .... i .... , .... , .... , ....... , .... , .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 %mjlt 2:C6 Sulfonate (PFHS) L34910-18, DF=100 073103A-1039 Sm (Mn, 2x3) 01-Aug-2003 23:11:3_ LC/MS/MS #E MRM of 4 Channels ES- 8.96 399 > 8(3 0'_, , , , .... , .... i .... i .... , .... , .... , .... i .... , .... , .... , .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 3:C8 Sulfonate (PFOS) L34910-18, DF=100 073103A-1039 Sm (Mn, 2x3) 01-Aug-2003 23:11:3_ LC/MS/MS #6 MRM of 4 Channels ES- 9.26 499 > 99 Area i 0 _l' %111_ [ 'l .... ' .... 2.00 ' .... I .... 4.00 I .... I .... 6.00 I .... I .... 8.00 I .... ' .... 10.00 ' .... ,Time 12.00 Ex1_en Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 PEinted: Sun Aug 03 07:19:29 2003 Page 78 Decatur BC BC 080103 Name: 073103A-I039 Text : 4 : PFOSA !L34910-I8,DF=I00 073103A-1039 Sm (Mn, 2x3) l nn_" 01-Aug-2003 23:11:3_ LC/MS/MS #_ MRM of 4 ChannelsES- 9.90 _ 12191 498 > 78 6.51e4 Area '" ' ' J .... I .... 2.00 I .... I .... 4.00 I .... "l .... 6.00 _ .... _ .... 8.00 , ....... 0.00 t .... ,lime 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:073103A, Ext.Date:07131/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals. PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07=19:29 2003 Page 79 Decatur BC BC 080103 Name: 073103A-1040 Text : i: C8 Acid (PFOA) XC072503-5, 500 ng/L Standard 073103A-1040Sm (Mn, 2x3) 100--] o,t i].... i_'_' , . , .... 2.00 , .... , .... 4.00 _I_ : C6 Sulfonate (PFHS) XC072503-5, 500 ng/L Standard 073103A-1040 Sm (Mn, 2x3) , .... , .... 6.00 9.12 156964- , .... t ....... 8.00 8.98 01-Aug-2003 23:33:24 LC/MS/MS #6 MRM of 4 ChannelsES413 369 9.33e5 Area , .... 10.00 , .... LTime 12.00 01-Aug-2003 23:33:24 LC/MS/MS #6 MRM of 4 ChannelsES399 80 : 1 11o/l 0 I, . . , .... _ .... 2.00 i .... _ .... 4.00 3:C8 Sulfonate (PFOS) XC072503-5, 500 ng/L Standard 073103A-1040 Sm (Mn, 2x3) i11i0-_ .... ,'"'''_ .... 2.00 _ .... , .... 4.00 , .... _ .... 6.00 _ .... ,.... 6.00 290381 1.78e5Area , .... , .... , .... , . . . , .... ,Time 8.00 10.00 12.00 01-Aug-2003 23:33:24 LC/MS/MS #6 MRM of 4 ChannelsES- 9.24 499 99 Area 193411 _ .... ,.... , .... i .... 8.00 10.00 1.13e5 _ .... _Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 _lantify Sa_le Report _ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\SampleDB\073103A Sun Aug 03 07z08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 80 Decatur BC BC 080103 Name: 073103A-I040 Text : 4 : PFOSA XC072503-5, 500 ng/L Standard 073103A-1040 Sm (Mn, 2x3) ' :.; _ 01-Aug-2003 23:33:24 LC/MS/MS #6 MRM of 4 ChannelsES- 9.90 498 > 78 Area ; 1i0_ 72430_ 3.86e5 1 YlI .... i .... _ .... _ .... _ .... _ .... i .... , .... '_ .... _ .... _ .... _ .... LTime 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 %_m4V Quantify Sample Study NO.:L34910, Report Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDBk073103A Sun Aug 03 07:08:13 2003 P:kData\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 81 Decatur BC BC 080103 Name: 073103A-I041 Text : i: C8 Acid L34910-25 (PFOA) 073103A-1041 Sm (Mn, 2x3) 01-Aug-2003 23:55:08 LC/MS/MS #6 MRM of 4 ChannelsES- 1.72e4 9.i 3 Area O'r,, ,'_,, .... _ ,-,_,,,,,, 2.00 %_ 2:C6 Sulfonate L34910-25 (PFHS) 073103A-1041 Sm (Mn, 2x3) 1000715 .36 o _j_'-- /_/_A"l"602"7_53"A07 ,-'2-'_,,, ,, ,., .... , .... , .... I .... ,',,, ,,Time 4.00 6.00 8.00 10.00 12.00 4"154"'6 5k51_'836_'0 01-Aug-2003 23:55:08 _ LC/MS/MS #6 . _11 MRM of 4 ChannelsES- 899033 399>__8o_ ..7_/_ 8,118_/_8/,,..11,,_11_2 /'3_ ' ' ' ' I .... I ' ' ' ' I ' ' ' ' I ' ' ' ' [ ' ' " ' I .... 2.00 4.00 6.00 3- C8 Sulfonate L34910-25 (PFOS) 073103A-1041 Sm (Mn, 2x3) I ' ' I I ] I ' ' I I ' ' ' ' I ' ' ' ' I .... 8.00 10.00 I 12.00 01-Aug-2003 23:55:04 ! LC/MSS #6I MRM of 4 Channels ES- I 9.22 499 > 99I V 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 _1_f Quantify Sample Report Study No.:L34910, Set No.=073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample LAst: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluor0chemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 82 Decatur BC BC 080103 Name: 073103A-I041 Text : 4 : PFOSA L34910-25 073103A-1041Sm (Mn,2x3) 100-_ 10.12 11.873"21 | 11-Aug-2L0C0/M3 S2/3M:S55:#068 MRM of 4 ChannelsES- 9.85 498 > 78 A 1.12e3 6.09 7.36 8 02 "' 1 7 11.30 1 Time 2.00 4.00 6.00 8.00 10.00 12.00 tq,,i Ex2_en Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set NO.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample LiSt: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\SamplsDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 83 Decatur BC BC 080103 Name: 073103A-I042 Text : i: C8 Acid (PFOA) L34910-26 073103A-1042 Sm (Mn, 2x3) 10 O] A // " " 913 02-Aug-2003 00:16:5_ LC/MS/MS #E MRM of 4 ChannelsES413 > 3691 1.93e4 Area .... , ' '" ' , .... 2.00 %_I 2:C6 Sulfonate L34910-26 (PFHS) i .... i .... 4.00 073103A-1042Sm (Mn, 2x3) 100-] 0.90/_ , .... i .... 6.00 , .... L .... 8.00 f .... i .... 10.00 , .... ,Time 12.00 02-Aug-2003 00:16:59 LC/MS/MS #6 I MRM of 4 ChannelsES- _! 9.42 399 >98200 6 16 7 76 8.08 8.98 10:21 1172 .... ,.... i'' "" i .... , .... ,...'._.... _,".',._ .... ,.... _.... , .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 3:C8 Sulfonate L34910-26 (PFOS) 02-Aug-2003 00:16:59 073103A-1042Sm (Mn, 2x3) 100_ _/ MRM of 4LCh/MaSnn/MeSlsE#S6- 9.27 499 99 A 1.55e3 .... , .... ,, .,., 2.00 .... , .... ,,, ..,, .... , .... , .... , .... _ .... , .... ,Time 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _|_ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 84 Decatur BC BC 080103 Name: 073103A-I042 Text : 4 : PFOSA L34910-26 . 073103A-1042.Sm (Mn, 2x3) 02-Aug-2003 00:16:59 LC/MS/MS #6 MRM of 4 ChannelsES- Area 0 I ,,, , .... = , , , . , .... i .... 2.00 4.00 , .... , .... 6.00 , .... _ .... 8.00 , .... , .... 10.00 4.77e3 ,. ,.. ,Time 12.00 V _ygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Sat No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: Pz\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals. PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07119=29 2003 Page 85 Decatur BC BC 080103 Name: 073103A-I043 Text : I: C8 Acid (PFOA) L34910-22 073103A-1043 Sm (Mn, 2x3) 02-Aug-2003 00:38:4E LC/MS/MS #6 MRM of 4 Channels ES- 2.10e4 Area ,, 9.15 0F. ,'T'T_,., ..... , , , , .... , .... 2.00 4.00 , .... ., ...........] .............I 6.00 8.00 8I 08 -- I 10.00 I Time 12.00 %_ 2:C6 Sulfonate L34910-22 (PFHS) 02-Aug-2003 00:38:4E 073103A-1043 Sm (Mn, 2x3) 10-- 0.89 _j MRM of 4LCCh/MaSnn/MeSlsES#6- 8.318.84 9.53 11.04 399 68_ : C8 Sulfonate L34910-22 2.00 (PFOS) 073103A-1043 Sm (Mn, 2x3) lOOn -t 0 92 1.27 " . " 4.00 6.00 8.00 , 6.90 _ 10.00 12.00 02-Aug-2003 00:38:4E LC/MS/MS #6 _ MRM of 4 ChannelsES- _V11 11"5-5_.. 499 > 99 9.28 ' 11.30 /_ 894 V 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No. zL34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19=29 2003 Page 86 Decatur BC BC 080103 Name: 073103A-I043 Text : 4 : PFOSA | L34910-22 073103A-1043 Sm (Mn, 2x3) 0S-Aug-2003 00:38:4E _/ LC/MS/MS #E MRM of 4 ChannelsES- 9.90 498 > 78 10C 0.26 1 24149 311 355 414 5.165..40 6.36 ...... 893 9'55/g_ 11.3,,211:70 621 " 2.69 " " " 4.74 6.85 /.44 o.,:, " C .... _ .... _ .... 2.00 , .... = .... 4.00 _ .... _ .... 6.00 , .... ..... 8.00 i .... i .... 10.00 , .... ,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L3_910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\O73103A Sun AuG 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun AuG 03 07:11:59 2003 Printed: Sun AuG 03 07:19:29 2003 Page 87 Decatur BC BC 080103 Name: 073103A-I044 Text : i: C8 Acid L34910-23 (PFOA) 073103A-1044 Sm (Mn, 2x3) ot 100_ 9.13 34004" 02-Aug-2003 01:00:38_ LC/MS/MS#6I MRM of 4 Channels ES- I 413 > 369I 2.09e5 Area -,. ,i,_r_"_, ,_ .... 2.00 _ .... _'"'' 4.00 2:C6 Sulfonate L34910-23 (PFHS) 073103A-1044 Sm (Mn, 2x3) 110-_ I .... I .... 6.00 _ .... I .... 8.00 , ,,-,, .... 10.00 _ .... _Time 12.00 8.91 6648- 02-Aug-2003 01:00:3_ LC/MS/MS #_ MRM of 4 ChannelsES399 > 80 4.02e4 Ares 0 I .... ',. '.., ,... '.,.. 2.00 3:C8 Sulfonate L34910-23 (PFOS) '..,. ,_-.. j .... , .... 4.00 6.00 073103A-1044 Sm (Mn, 2x3) , .,. '.. , ....... 8.00 9.24 ,. ,-,., .... ,Time 10.00 12.00 02-Aug-2003 01:00:3E LC/MS/MS #(3 MRM of 4 ChannelsES499 > 99 0-_ ......,............,.......... , _ _ , , , : , . . ......i.... , _Time 2.00 4.00 6.00 8.00 10.00 12.00 Exy_en Research, 3058 Research Drive, State ColleGe, PA 16801 Quantify Ssm_le Report _ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Rieha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 88 Decatur BC BC 080103 Name: Text: 073103A-I044 4: PFOSA L34910-23 073103A-1044Sm (Mn, 2x3) 02-Aug-2003 01:00:38 LC/MS/MS #6 MRM of 4 ChannelsES- 9.89 498 > 78 111 .... i.... ,.... i.... J .... ,.... ,.... , .... , .... i12140_ L .... , .... ,6T.A4i5rmeeea4 !: 2.00 4.00 6.00 8.00 10.00 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.=073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified= Method: Last modified: Job Code= P:kData\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 89 Decatur BC BC 080103 Name: 073103A-I045 Text : i: C8 Acid (PFOA) L34910-24,DF=100 073103A-1045Sm (Mn, 2x3) 02-Aug-2003 01:22:1 ! LC/MS/MS #6I MRM of 4 ChannelsES- I 9.13 413 > 369I 11/1 35258_ 2.06e5Area 1 0 _ , , ,_, , , I .... 'l '" ' ' _ .... I .... _ .... _ .... I .... i .... "i '" ' ' _ .... 1Time 2.00 4.00 6.00 8.00 10.00 12.00 %_ : C6 Sulfonate (PFHS) L34910-24,DF=100 073103A-1045 Sm (Mn, 2x3) 02-Aug-2003 01:22:I LC/MS/MS #6 MRM of4 ChannelsES- 8.96 399 > 80 11o/,1 0"-...,,,-, . . , .... 2.00 3:C8 Sulfonate (PFOS) L34910'24, DF=100 i-= . . , , .... 4.00 073103A-1045 Sm (Mn, 2x3) , .... _ .... 6.00 60021 , .... , .... _ .... , .... 8.00 10.00 3.3A9rea4 , .... ,Time 12.00 02-Aug-2003 01:22:1(] LC/MS/MS #6 MRM of 4 ChannelsES- 9.25 499 > 99 Area 1i0-_ i_._, V .... .., .... 2.00 , . . .'. , .... 4.00 , . . . ,.', .... 6.00 38531 , . .'; . ,_ . . . , . . .'. , .... 8.00 10.00 2.26e4 , .... ,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _mJ Study No.:L34910, Set No.:O73103A, Ext.Date:07131103, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\Sam_leDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Stul Aug 03 07:19:29 2003 Page 90 Decatur BC BC 080103 Name: 073103A-I045 Text : 4 : PFOSA L34910-24,DF=I00 073103A-1045 Sm (Mn, 2x3) 11(7_ 02-Aug-2003 01:22:10 LC/MS/MS #6 MRM of 4 ChannelsES- 9.89 498 > 78 16047- Area _ 8.50e4 1 i .... , .... , .... , .... _ .... , .... j .... _ .... ', .... , ..... ',,, .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 qlW Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %qJ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Su_ Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 91 Decatur BC BC 080103 Name: 073103A-I046 Text : i: C8 Acid (PFOA) XC072503-6, 1000 ng/L Standard 073103A-1046 Sm (Mn, 2x3) 100-] 9.13 322068- 02-Aug-2003 01:43:42_ LC/MS/MS #6 l MRM of 4 Channels ES-] 413 369I 1.93e6 Area .... , .-... _ .... , .... , .... , .... _ .... , .... , .... _ _. . . , .... , .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 %_ 2:C6 Sulfonate (PFHS) X0072503-6, 1000 ng/L Standard 073103A-1046 Sm (Mn, 2x3) 02-Aug-2003 01:43:42 LC/MS/MS #6 MRM of 4 ChannelsES- 8.98 399 80 1iC .... _.... , .... 2.00 , .... , . . . . , .... , .... 4.00 6.00 3:C8 Sulfonate (PFOS) XC072503-6, 1000 ng/L Standard 073103A-1046 Sm (Mn, 2x3) , .... , 6..0..9411, .... , .... 8.00 10.00 , .... ,3T.i7m1eAreae5 12.00 02-Aug-2003 01:43:42 LC/MS/MS #6 MRM of4 ChannelsES- 9.24 499 99 Area i qm, 0 '.._., .... , .... 2.00 , .... , .... 4.00 , .... , .... 6.00 , .... , .... 8.00 , .... ,..'.,, 10.00 .... ,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Queultify Sample Report _ Study No.:L34910, Set No.:073103A, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103A Sun Aug 03 07:08:13 2003 P:\Data\LCMSMS6\Maselynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:19:29 2003 Page 92 Decatur BC BC 080103 Name: 073103A-I046 Text : 4 : PFOSA XC072503-6, I000 n_h Standard 073103A-1046 Sm (Mn, 2x3) 02-Aug-2003 01:43:42 LCIMS/MS #6 MRM of 4 ChannelsES- 9.89 498 > 78 11=/1 139302J- _ 7.3A8rea5 1_ 0 I .... _ .... , .... , .... i .... i .... , .... , .... L .... , ....... 4 .... ,Time 2.00 4.00 6.00 8.00 0.00 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 _,_mJ q_ Sponsor Study No: Exysea Study No: Anslyts: Ions Mouhmnd: Site: NA !..34910 PFOA 413 -> 369 _mr Baker's Czeck RAW DATA REPORT L/mit of Quanfitafion: Injectioa Volume: Malxix: Sample Volume: Final Volume: 50 ppt 15 I.tL Water 40.0 mL 5.0 mL Set No: Analyst: InstrumentType: Extraction Date: Analyzed on: 073103AR Katen Risha LC/MS/MS Unit # 6 07/31/03 08_3-O4/03 Exygen ID XC072_03-0 XC072503-1 XC07_03-2 XC072_03-3 XC077..503-4 XC077.503-5 XC072503-6 L34910-1 SpkC L.34910-12Spk E L349[0-16 Spk F XC072503-! 1..34910-I L34910-_ Rep L34910-4 L34910-2 XL-_72503-2 L34910-6 Sponsor . [13 - BC2 SW..04 BC2 SW-06 Outfalt to River SW-25 BC2 SW-04 BC2 SW434. BC2 SW-04 Dup BC2 SW-04 Low _qpk BC2 SW-05 Sample Code CS CS CS CS CS CS CS Lc, LF LF CS $ S $ FF CS $ Run No. 073103AR-I01 073103AR-102 073103AR-103 073103&R-t04 073103AR-105 073103AR-106 0"/3Ia3 b.R-].07 073103AR-108 073103AR-I09 if'/31Q3AR-t 10 073103AR-111 073103AR-112 073103AR-113 073103AR-I14 073103AR-I 15 073103AR-116 073103AR-117 $td. Conc. ([_t) 0 25 50 I_ 2_0 500 1000 25 50 Dilution Factor 100 100 10(3 10 10 I0 10 10 Peak Area 794 14221 27994 54680 128556 264862 516215 50564 92540 114710 14631 21604.1 216268 131415 142555 29284 40498 L34910-6 Rep 1.34910-9 1.34910-7 XC072503-3 L34910-12 L3_.910-12 Rep L,_910-15 1.34910-13 XC077.$03-4 L34910-16 L34910-16 Rep 1.34910-19 1.34.910-17 XCff725_-5 1,34910-16 I..34910-16 Rep L34910-19 L3d,910-17 XC071003-.6 BC2 SW-05 BC2 SW-05 Dup BC2 SW-05 Low Spk BC2 SW-06 BC2 SW-06 BC2 $W-06 Dup BC2 SW-06 Low Spk Ouff'a].lto River SW-2_ Ouffall to River SW-25 OuffaU to River SW-25 Dup Outfall to River SW-2_ Low Spk Outfall to River SW-2_ Outfall to River SW-25 Outfall to River SW-25 Dup Outfal| to River SW-25 Low Spk S S FF CS S S $ FF CS S S S FF C.S S $ ,S FF CS 073103AR-118 073103AR-119 073103AR-120 073103AR-121 I00 073103AR-122 073103AR-123 -. 073103AR-124 073103AR-125 073103AR-126 073103AR-127 . 250 073103AR- 17.8 073103AR-129 073 I(DAR-130 073103AR-131 _0 073103AR-132 073103AR-133 073103AR-134 073103AR-135 073103AR-|36 1000 Analy_c Found (ppt) : (peak area - intet_,,ept/) slope x DF Recovery (%) : [analytc found (ppt)-anal_c found in control (ppt)] x ICO amount added (ppt) 10 39782 10 81652 10 112700 55667 20 308911 20 315651 20 297735 20 354730 127797 I00 82515 100 83658 100 75424 100 78536 271906 20 380900 20 391789 20 364595 20 362898 477931 Analyte Found Ippt) Amount Added (p[Jt) Recovery I%) ** 17800 221(30 4210 4210 2540 2760 ** ** 1560 2170 12100 12300 11600 13900 15800 16000 14_t00 15000 ** ** ** ** 5000 5(200 .f_00 100 100 100 100 100 114 126 -1450+ 1579A+ 1800+ 400+ Sctndurd _e : Linear (1/x weighted) Inmrccpt : 2202.17 Slope : 508.394 Cc_f. Of Det.= 0.996211 CS Calibration standard LF : Lab fortified sample C = Cou_roslample S = Smnple CK _*Check Sumdatd FF : Fieldfortifiteadmple I..CS: Laboratory Coum01Spike ND = Not dutectcd = Respcmanbetween 0 and25 ppt NQ : Not quantifiable : Response between 25 pptand LOQ (50 ppt) i_ Spreadsheet prepared by: r4_i_).3 **Sample was analyzcd with se'vcrald_inlionfac_m'sin order to accommodate all _nds. The appropriateresults are reported. ^Sample was coaecmd using the data found in set 073103A. +_.gampleresidue slgnifieandy exceeds the spikin8 level; therefore, an accurate recovery caanot be calculated. %m9' Spommr Study No: Exygeu Study No: Aaaly_e: Ions Moeimred: Site: NA L34910 PFHS 399 -> 80 Decatur Baker'sCreek RAW DATA REPORT limit of Quaatitadon: lnjecfiou 'Volume: Matrix: Sample Volume: Fma]Volume: 50 ppt 15 }JL Water 40.0 mL 5.0 mL Set No: Analyst: ImtmamentType: Extraction Dam: Analyzed on: 073103AR Karen Ri,ha LC,/MS/MSUnit # 6 07/31/03 08/03-04/03 Std. Amdyte Amount Exygen Spomo Sample Rue Cone. Dilution Peak Found Added Recover,/ lD XC072503-0 113 Code No. (pp0 Factor Area {ppt) (pin) (_) CS 073103AR-101 0 0 XC072503-1 XC0"/2503-2 CS 073103AR-102 25 C,$ 073103AR-103 50 2074 4715 XC072503-3 CS 073103AR-104 100 9231 XC077.503-4 XC072503-5 CS 073103AR-105 2_0 CS 073 I03AR-106 500 21488 43819 XC077.503-6 CS 073103AR-107 10(]0 87115 I,.34910-1 Spk C L34910-12 Spk E _910-16 Spk F BC2 SW-04 BC2 SW-06 Out'fallto River SW-?.5 LF 073103AR-108 " LF 073103AR-109 LF 073103AR-! I0 100 5566 ** 5000 100 10314 11800 _ 115 100 10701 12200 5000 91 XC072503-1 CS 073103AR-I 11 25 2324 L34910-1 BC2 $W-04 $ 073103AR-! 12 10 9381 *" 4 L34910-1 Rep BC2 SW-04 S 073103AR-113 i0 10152 ** 1.34910-4 ' BC2 SW-04 Dup S 073103AR-114 10 6122 *" L34910-2 XC072503-2 BC2 SW-04 Low Spk FF 073103AR-115 : 10 7036 ** 100 CS 073 I03AR-116 50 4266 L34910-6 BC2 SW-05 $ 073103AR-117 10 1526 ** qh_lV L.34.910.6 Rep BC'2SW-05 S 073103AR-118 10 1565 "* L34910-9 BC2 SW-05 Dup S 073103AR-119 10 3729 ** - 1,34910-7 XC'O72_03-3 BC2 SW-05 Low Spk FF 073103AR-120 10 6025 ** 100 CS 073103AR-121 100 9486 L34910.12 1.34910-12 Pep BC'2SW*06 BC"2SW-06 $ 073103AR-122 S 073103AR-123 20 26169 6060 20 27209 6300 i.34910-15 BC2 SW-06 Dup S 073103AR-124 20 25364 5870 L34910.13 XC072503-4 BC2 SW-06 LOw Spk FF 073103AR-12.1 20 30673 7110 100 1050+ CS 073 I03AR-126 2_0 21551 /.,34910.16 Oulfnil to Rivet"SW-25 S 073103AR-127 100 6872 ** L34910-16 Pep i.34910-19 Oulfall m River SW-2._ (Xtu_,fito River Sw-2.S Dgp $ 073103AR-128 S 073103AR-129 100 6261 ** 100 6156 "* 1,34910-17 XC072503-5 1-34910-16 Outfall to River SW-25 Low Spk FF 07311DAR-130 100 6030 ** 100 CS 0'73103AR-131 500 45496 Outfall to River SW-25 S 073103AR-132 20 33004 7660 L34910-16 Rep Outfall m Ri'vetSW-2_ S 073103Ag-133 20 30633 7100 1,34910-19 L34910-17 XC071003-6 Outt'all m River SW-7.$ Dep Outfall to River SW-7.5 Low Spk S 073103AR-134 20 FF 073103AR-135 20 CS 073103AR-136 1000 29219 6770 28660 6640 80818 100 -1020+ Amdyle Found (ppt) = (peak area - inte_'tX) I slope x DF Recovery (%) = [anal]rtefound (ppt)-anad?',"found in control (ppt)} x 100 amount added (ppt) S_d Curve : Linear (I/x weighted) Inmrre,lx = 218.845 Slope =, 85.6521 Coef. Of Det. = 0.99_60 CS = Ca, libra6on $taJadard LF = Lab fozlified sample 'q S = Sample CK = Check Smadard LCS = Laboratory Cona, ol Spike ND = Not detected = Respome between 0 aad 25 ppt 5pre_d_a_t Ixepaz_.__::l ,,_ 0"_. O_ ' _) V NQ = Not quamifiable = Kespon._ betweea 25 pptand LOQ (50 ppt) **Sample w_ analyzed with several diludon factors in order to ar.commndateall compounds. The apl_3priamresul_ are reported. +Sample residue significaady exceeds the spiking level; therefore, an accurate recovery cannot be calcalated. i ii sponsor Study No: Exygen Study No: Analyte: lent Monitored: Si_: NA 1.34910 PFOS 499 -> 99 DecaturBaker'sCreek RAW DATA REPORT Limit of Quandtafioa: Injccden Volume: Mauix: Sample Volume: F'uudVolume: 50 ppt 15 pL Water 40.0 mL 5.0 mL Set No: A_dy_ Insmm_ut Type: Extraction Date: Amdyzedon: 073103AR Kare'__a LC/MS/MS Unit # 6 07/31/03 08/03-04/03 Std. Analyte Amount Exygea Sponsor Sample Rua Couc. Dilution Peak Found Added Recovery ID XC(T/2.q)3-0 XC072_03-! ID Code No. (ppt) Factor Area (ppt) (ppt) (%) CS 073103AR-10I 0 0 CS 073|03AR-102 25 1481 XC077.503-2 CS 073103AR-103 50 2986 XC072503-3 - XC07_-4 CS 073103AR-104 100 CS 073103AR-10$ 250 5100 13285 XC072503-5 CS if'/3103AR- 106 500 28978 XC072503-6 CS 073103AR-107 10O0 53617 L34910-1 SpkC L34910-12 Spk 1_ L34910-t6 Spk F XC077.503-I BC2 SW-04 BC2$W-06 Outfall to River SW-25 LF 073103AR-108 100 9428 17100 50(]0 112^ LF 073103AR-109 100 17124 ^^ 5000 LF 073103AR-I 10 1()0 22403 _'_ 5000 CS 0"/3103AR-I11 25 1473 L34910-1 BC2 SW-04 $ 073103AR-112 10 61501 * 1.34910-1 pep BC2 SW-04 S 073103AR-113 10 59888 * 1.34910-4 BC2 SW-04. Dup S 073103AR-114 10 44921 _250 L34910-2 XC072503-2 BC2 SW-04. Low Spk FF 073103AR-115 CS 073103AR-I 16 50 10 37560 6890 2882 100 -461(P+ I..34910-6 BC2 $W-05 S 073103AR-117 10 9224 1670 LM910-6 pep 1,34910-9 BC2 SW-O5 BC2 SW-O5 Dup S 073103AR-118 S 073103AR-119 10 8484 1540 10 23649 4330 _l_ L.34910-7 BC2 SW-05 Low Spk FF 073103AR-120 10 29284 5370 100 3700+ XC072503-3 CS 073103AR-121 I00 6004 L34910-12 BC2 SW-06 S 073103AR-122 "20 64499 * L34910-12 pep L34910-15 L34910-13 XC072503-4 BC2 SW-06 BC2 SW-06 Dep BC2 SW-06 Low Spk $ 073103AR- 17.3 20 64047 * S 073103AR-124 *, 20 64656 * FF 0731D3AR-125 20 77839 * I(X) CS 073 [03AR-125 250 13289 L34910-16 Outfall to River SW-25 S 073103AR-127 100 17094 31200 L34910-16 Rep Ouffallto River SW-25 S 073 I03AR-128 100 17264 31500 L34910-1.9 L34910-17 XC072503-5 (3utfsl[ to RbRx SW-25 Dup $ 073103AR-t29 100 16861 30800 Outfall to River SW-25 Low Spk FF 073103AR-130 100 16123 29400 100 .1800+ CS 073103AR-131 500 28469 L34910-16 L34910-16 Pep Outfall to River SW-7.5 Outfall to River SW-28 $ 073103AR-132 S 073103AR-133 20 81862 ** 20 84263 ** 1.34910-19 Ottffallto River SW-28 Dup S 073103AR-134 20 827.,01 ** I..34910-17 Ouffall to RiverSW-25 Low Spk FF 073103AR-135 20 79698 ** 100 XC071003-6 CS 07310tAR-136 1000 531.57 AJlalyteFound (PP0 = (peak area. ialetcept) I slope x DF Recovery (%) = [analyte found (ppt)*analytefound in control (ppt)] x 100 amount added (ppt) S_dard _e : Lineal (lht weighted) hitercept ffi 152.345 Slope = 54.2_82 Conf. Of DeL = 0.998217 CS = C.aliMadoastemLard LF = Lab fortified wn, ple C ffi Coulxoixa, mp_ S ffiSample CK = Check Standard FF= _eld fortifiedsample LCS = Label,aloe/Coutrol Spike ND = Nee detected = R_ between 0 and 25 ppt NQ = Not quandfud_le = R_poase between 25 ppt and LOQ (30 PP0 Spread._eet prepmnd by: d_ _ ]..- [_._ _I_ .**Sampln w= _mniy=dwi_ =vend di]ndonfactor* in orderm accommodateMI compoundsT.he appropriateresul_ are =porled. ^Sample wet corm=ted udng the data found in set 080603A Sample xequh_ ruddereh'ludoa.See data _:t 080603A "Sample requires a higher spildn8 level. See data set 080603A. +Sample residee siSnificaady exceed_ the ipikni$ level; _erefot'e, aa accuraterecovery ctaao_ be calculated. Sponsor Study No: ExygenStudyNo'. Analyte: Ions Monitored: Site: NA 12,4.910 FOSA 498 *>78 Decatur Baker's Creek RAWDATAREPORT Limit of Quantisation: In_ectionVoltaire: Matrix: Sample Volume: Final Volume: 50 ppt 15 p.L Water 40.0 mL 5.0 mL Set No: Analyst: Ins[rim'[cutType: Extraction Date: Analyzed on: 073103AR Karen Risha LC/MS/MS Unit # 6 07/31/03 08/03-04/03 Std. Analyt_ Amount Exysen Sponsor Sample Run Cone. Dilution Peak Found Added Recovery ID XC072503-0 ID Code No. (ppt) Factor Area (ppt) (ppt) (%) CS 073103AR-101 0 0 XC072503-1 CS 073103ARo102 25 5175 XC072503-2 XC072503-3 CS 073103AR-]03 50 CS 073103AR-104 100 10303 20719 XC072503-4 CS 073 i03AR-105 250 48632 XC072503-5 CS 073 I03AR-106 500 104085 XC072503-6 CS 073103AR-107 1000 196920 L34910-1 Spk C BC2 SW-04 LF 073103AR-108 100 13039 ** 5000 L34910-12 Spk E BC2 SW.06 LF 073 I03AR*I09 100 16006 ** 5000 L34910-16 Spk F Outfall to River SW-25 LF 073103AR-110 100 18398 ** 5000 XC072503-1 L34910-1 BC2 SW-04 CS 073103AR-111 25 5382 S 073103AR-112 10 27920 1390 1 L34910-1 Rep BC2 SW-04 S 073103AK-113 10 27505 1370 L34910-4 BC2 SW.04 Dup S 073103AR-114 10 20497 ** L34910-2 XC072503-2 L34910-6 BC2 SW-04 Low Spk BC').SW-05 FF 073103AR-115 IO 16630 ** IOO CS 073103AR-116 50 10890 S 073103AR-I 17 IO 3460 ** L34910-6 Rep L34910-9 1.24910-7 XC072503-3 1.34910-12 L34910-12 Rep L34910-15 L34910-13 XC072503-4 L34910-16 L34910-16 Rep L34910-19 L34910-17 XC072503-5 L34910-16 L34910-16 gep L34910-19 1.34910-17 XC071003-6 BC2 SW-O5 BC2 SW-05 Dup BC2 SW-05 Low Spk BC2 SW.06 BC2 SW-06 BC2 SW.06 Dup BC2 SW.06 Low Spk Ouffall to River SW-25 On[fall to River SW-25 Ouffall to River SW-25 Dup OutfaUto River SW-25 Low Spk On[fall m River SW-25 Ouffall to River SW-25 Ouffall to River SW-25 Dup Outfall to River SW-25 Low Spk S 073103AR-118 S 073103AR-119 I0 3402 ** IO 8876 ** FF 073103AR-120 I.O 11595 *" CS 073103AR-121 100 21221 S 073103AR-122 20 24495 2430 S 073103AR- 123 20 23261 2300 S 073103AR.124 20 25908 2570 FF 073103AR-125 20 25736 2550 CS 073103AR-126 250 49195 S 073103AR-127 100 6718 ** S 073103AR-128 100 6206 ** S 073103AR-129 100 6506 ** FF O73103AR-130 1OO 5831 ** CS O73103AR-131 500 102292 S 073103AR-132 20 32659 3260 S 073103AR-133 S 073103AR-134 20 31916 3180 20 32869 3280 FF 073103AR-135 20 26767 2660 CS 073103AR.136 I00_ 190680 IOO 100 120 IOO I00 .600+ Analyte Found(ppt) = (peak area - intercept) / slope x DF Recovery (%) - [analySe found (ppt)-analyte found in control (ppt)] x 100 arnountadded (ppt) StandardCurve : Linear(l/x weighted) Intercept - 611.080 Slope = 196.925 Coef. Of DeS.= 0.998392 CS = Cal_rtdon standard LF = Lab fortified sample CS ==SCamonpUle'olsample CK = Check Standard FLFCS- =FLiealbdofroarttoirfyieCdosnamtxoplleSpike ND - Not detect_l = Response between0 tnd 25 ppt NQ = Not quantit'utble= Response between 25 ppt and LO_ (50 PP0 Spreadsheet prepared by: ._ **Sample was analyzed with seven[ dilution factors h order to accommodate aUcompounds. The zppmpr/ale results are reported. +Sample residue significantly exceeda the spiking level; therefore, an accurate recovery cannot bc calculated. ^O,_t_J_ = ke 2 3| 5 .oocoo co c- ove- 23R8 e 2288 8 se8 ss. FoEe occccoccccoccoscscsscssosssssssesss TTT ETT ETRY TETTTRECTTTRORTRUTRNRORY lg 95 one278888A8a1 118011188, 1 80,1186, 88o g s| F|i! s 1 333s333sBt 25s i B Ftrehei eBlJiagal s lEBiFae tseaBlJi oissaB | Fonnmnmnnnnnning i "log8 || Sisf8 rz 3 3% d2l333e545d8 13 1110 iEl lsEhmL nigiL iigEleslsetistitLn d : | fa 585853833959333033930838308R33583385 | 82 Q & 2 Pol Eoin 3 s3s3sssasecazzesssennunInaNanazanany Hy 39) I seszzeeicecifseiiscrisanizznEazes -t i 5 2 IYoISeTNRYIRELUBR8SIUBIBIBERBIRANAY ii rNovwenea2rNOTLLESeRRNARREREREENRIRG ,,= _, o ':E_ 0 n o) (3. ILl o o_ __ _ E mmmmmmm_mmmm_mmmmmmmmmmm . EE________ _ mm mmmm mm m ==== o== = ==_ =====ooooooo o __ __ <<<<<<<<<<<_<<<<<<<<<<<<<<<<<<_<<< 000000000000000000000000000000000000 O0 0000 000 _=_ ========================= oo 000000_0000000000_0000_0000000000000 LC/MS/M_S SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exygen Study No: L34910 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #6) Computer: Software: COMPAQ Professional Workstation AP200 Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 HPLC Equipment: Hewlett Packard (I-IP)Series 1100 HP Bin Pump I-IP Vacuum Degasser I-IPAutosarnpler HP Column Oven HPLC Column: Genesis C-8, 5 cm x 2.1 mm i.d. x 4 _t (Exygen ID: 74A) (JONESCHROMATOGRAPHY: Part No. FK5962E) Mobile Phase (A) : 2 mM Ammonium Acetate in Type I Water MAnoabliylset:Phase (B) : MKaertehnanRoilsha __/(_ ! Exygen Research 3058 Research Drive, State College, PA 16801 ql_ Phone: (814)272-1039 FAX: (814)231-1580 NOTE: The next 3 pages are computer generated printouts from the masslynx software program. The pages contain the instrument settings used for the analysis of this data set. All HandwriUen Peak ID's by: _!0_10_ V %_ Scanning Method Report Method: Last Modified: C:\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\C6 Thu Jul 31 16:23:50 2003 C8 SULF C8 ACID PFOSA Page 1 Printed: Sun Aug 03 08:20:40 2003 _l_I_ Solvent Delay ( mins ) : 0.00 Analog Channel Function :1 4 : Unused MRM of 4 Mass Pairs ( ESP- ) Inter Channel Delay ( Secs ) : Span ( Daltons ): Start Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 12.00 1 Dwell 1 399.00 80.00 0.20 2 413.00 369.00 0.20 3 498.00 78.00 0.20 4 499.00 99.00 0.20 (Secs) Coll Energy 35 I0 30 40 _ (eV) Cone 50 iO 50 30 (V ) 4_ V Method Report Method File: Last Modified: C:\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\pfbs Sunday, August 03, 2003 08:06:07 water Page 1 _ Printed: HPII00 LC Pump Initial Conditons Solvents A% B% C% D% Sunday, August 03, 2003 08:20:45 90.0 10.0 0.0 0.0 _10_ Flow (ml/min) Stop Time (mins) Min Pressure (bar} Max Pressure (bar) Oven Oven Temperature Temperature Left(C) Right(C) 0.300 20.0 0 400 35.0 35.0 HPII00 LC Pump Gradient Timetable The gradient Timetable contains 8 entries which are : Time 0.00 2.00 5.00 9.00 9.50 14.00 14.50 20.00 A% 90.0 90.0 i0.0 10.0 0.0 0.0 90.0 90.0 B% I0.0 i0.0 90.0 90.0 I00.0 i00.0 10.0 I0.0 C% D% Flow 0.0 0.0 0.300 0.0 0.0 0.300 0.0 0.0 0.300 0.0 0.0 0.300 0.0 0.0 0.300 0.0 0.0 0.300 0.0 0.0 0.300 0.0 0.0 0.300 HPIIQ0 LC Pump External Event Timetable The Timetable contains 6 entries which are : Time Initial 0.00 0.05 0.10 11.90 12.00 Column Switch Off Off Off Off Off Off Contact1 Off On Off Off Off Off Contact2 Off Off Off On Off Off 'Contact3 Off Off Off Off On 'Off Contact4 Off Off Off Off Off Off HPII00 Autosampler Initial Draw Speed Eject Speed (_i/min) Draw Position (mm) Stop Time (mins) Injection Volume(_l) Vial Number Conditions 200.0 200 0.50 20.00 15.0 27 Pressure 400 400 400 400 400 400 400 400 V _i_ Tuning Method Keport Me t_hod : C :\MAS SLYIqX\ FLUOROCHEMI CALS. PRO\ACQUDB\ FLUOROCHEMS Page 1 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapo!e 2 Source Block Desolva:ion Temp. Temp. Pressures Analyser Gas Cell Vacuum Set 3.00 20 0.0 0.O 0.0 i00 300 Rdbk -2.93 -15 i00 299 Rdbk OFF 4.2e-3 AnalYSer LM Res 1 HM Res i 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 8 - 15 9 2 ii 14.0 14.0 2.0 650 -647 Rdbk 135.1 767.4 Quantify Calibration Report Study No.:L34910, Set NO.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Calibration: P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\CurveDB\073103AR Printed: Wed Aug 06 11:03:59 2003 Compound I name: C8 Acid (PFOA) Coefficientof Determination:0.996211 Calibrationcurve:508.394" + 2202.17 Response type:Extema Std,Area Curve type:Linear,Origin:Exclude, Weighting: I/x,Axis trans:None Page 1 Decatur BC I- 1 (2 V n 0.0 200.0 400.0 600.0 800.0 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Calibration Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Calibration: Last modified: Printed: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\073103AR Tue Aug 05 07:03:45 2003 Wed Aug 06 11:03:59 2003 Compound 2 name: C6 Sulfonate (PFHS) Coefficient of Determination:0.996560 Calibration curve: 85.6521* x + 218.845 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: l/x, Axis trans: None 8.71e4- Page 2 Decatur BC x 4 Response- V 0 .... 0.0 , .... , .... 200.0 r .... , .... 400.0 , .... , .... 600.0 , .... , .... 800.0 , .... ,ng/L 1000.0 Exygen Research, 3058 Research Drive, State College, PA 16801 Q_antify Calibration Report _ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Calibration: Last modified: Printed: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\073103AR Tue Aug 05 07:03:45 2003 Wed Aug 06 11:03:59 2003 Compound3 name: C8 Sulfonate (PFOS) Coefficient of Determination:0.998217 Calibration curve: 54.2582 * x + 152.345 Responsetype: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: l/x, Axis trans: None Page 3 Decatur BC 0.0 200.0 400.0 600.0 Exygen Research, 3058 Research Drive, State College, PA 16801 800.0 ng/L 1000.0 Quantify Calibration Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Calibration: Last modified: Printed: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\073103AR Tue Aug 05 07:03:45 2003 Wed Aug 06 II:03:59 2003 COmpound4 name: PFOSA Coefficient of Determination: 0.998392 alibration curve: 196.925* x + 611.080 esponse type: External Std, Area :Curvetype: Linear, Origin: Exclude,Weighting: l/x, Axis trans: None 1.98e5- Page 4 Decatur BC _q,,# Response 0 ' ' ' ' _ .... , .... 0.0 200.0 _ .... , .... 400.0 , .... , .... 600.0 L ' ' ' ' , .... 800.0 _ .... i ng/L 1000.0 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified= Method: Last modified: Job Code: Printed: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Tue Aug 05 06=59:53 2003 P:\Data\LCMSMS6\Massllrnx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 I)_ _ _ Date O_lbf</o_ v Wed Aug 06 ii:04:02 2003 Run#____ToO__ Page 1 Decatur BC BC 080103 Name: 073103AR-101 Text : 1:C8 Acid (PFOA) XC072503-0, 0 ng/L Standard 073103AR-101 Sm (Mn, 2x3) 1,i,!n_.,_, ' ' ' ........ _.t 2.00 ' ' ' ' ' ' ' ' _ .... I '_ 4.00 6.00 2:C6 Sulfonate (PFHS) XC072503-0, 0 ng/h Standard 073103AR-101 Sm (Mn, 2x3) 1,,,_ 0.92 03-Aug-2003 19:10:54 LC/MS/MS #6 MRM of 4 ChannelsES- 3.99e4 Area 9.13 794 I ' ' ' ' I ' ' ' ' I ' ' ' ' I ' "' ' ' I .... 413I T>im3e69 8.00 10.00 12.00 03-Aug-2003 19i10:54{ 1 MRM of 4LCh/ManSn/MelSs E#S6-r1 8.99 399 > 801 uu-_ 043 A I_ 4 o/J_ ] / / \ 217 2.85 3.49405 4.665.43 =_,, 6.73 7.39 8.722A_'2%.59 11.12,, 4_ 797' -,o /XJ _A_ ,_ A A ,5"" " 2.00 4.00 3 : C8 Sulfonate (PFOS) XC072503-0, 0 ng/L Standard 073103AR-101 Sm (Mn, 2x3) 100-1 1.27 6.00 8.00 oo 1"09"_ ]/ =/01017 /V/ 2.15 2.48 3.05 348 A,I_ 5.37 6 "73 A ......... 10.00 12.(30 03-Aug-2003 19:10:5Zl LC/MS/MS #(3 i MRM of 4 ChannelsES- | 499 > 99 1.69e3 92 4 111"6 /'%, 10.1.21046 A 11.83 r_l " 0 .... , .... , .... , .... " -,.-,-, , .... , .... , .... i.uo f._4 , .... _._" , .... , .... " , .... ' .... ] Time V 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify SamPle Report _j_ Study No.:L34910, Set No.:073103AR, Ext.Date:07131103, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochercicals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 2 Decatu_ BC BC 080103 Name: 073103AR-I01 Text : 4 : PFOSA XC072503-0, 0 ng/L Standard 073103AR-101 Sm (Mn,2x3) 10C 0.751 ..... \_.UU1.17 2. 1 4 300 451480--^641 716.7.39 3.97 b.t_z " \ " _/_ 03_Aug-2003 19:10:54 LC/MS/MS #6 MRM of4 ChannelsES- 10.02 498 > 78 844876 9.21 A ". "_ /. it 109611.40 _" .< 572 11.83 C .... , .... , .... 2.00 _ .... , .... 4.00 , .... , .... 6.00 , .... _'-..''.., 8.00 .... ,..'.,, 10.00 .... ,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report ,_ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst=E.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDBk0?3103AR Tue Aug 05 06:59:53 2003 P:kData\LCMSMS6\Masslynx\Fluorochemulcals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 3 Decatur BC BC 080103 Naune : 073103AR-I02 Text : i: C8 Acid (PFOA) XC072503-1, 25 ng/L Standard 073103AR-102 Sm (Mn,2x3) . . 03-Aug-2003 19:32:33 LC/MS/MS #6 MRM of 4 ChannelsES- 14221- 8.87e4 Area ; 0,-_-_, ..... -..-, .... 2.00 , .... ,-, , r, , 4.00 , ' i c.. , w ' ' ' ' , ' : 7 .... , .... 6.00 8.00 10.00 ,,-.-'-_-_--'.,T, ime 12.00 _ 2:C6 Sulfonate (PFHS) XC072503-1, 25 ng/L Standard 073103AR-102 Sm (Mn,2x3) 8.98 2074 03-Aug-2003 19:32:33 LC/MS/MS #6 MRM of 4 ChannelsES399 > 80 1.28e4 Area 0_7--',_, , ,.... , .... 2.00 4.00 3:C8 Sulfonate (PFOS) XC072503-1, 25 ng/L Standard 073103AR-102 Sm (Mn, 2x3) 10(}] j'.... ,.... 6.00 ,.... , , : : ..... 8.00 9.24 1481] I =.... 10.00 , .... =Time 12.00 03-Aug-2003 19:32:33 LC/MS/MS #6 MRM of 4 ChannelsES499 > 99 8.99e3 Area .... I .... r .... , .... _ .... J .... i .... I .... J .... I .... _ .... I .... "iTIme 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 II Quantify Sample Report _ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 4 Decatur BC BC 080103 Name: 073103AR-I02 Text : 4 : 9FOSA XC072503-1, 25 ng/L Standard 073103AR-102Sm(Mn,2x3) 03-Aug-2003 19:32:33 LC/MS/MS #6 MRMof 4 ChannelsES- 9.90 498 > 78 o L.... _ , , , _j , , _', _, _ .... 2.00 4.00 _ .... _ .... 6.00 _ 'r' _' I .... "'_.......J k._ 8.00 10.00 _ .... _Time 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set NO.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:kData\LCMSMS6\MasslynxkFluorochemicals.PR0\Sam_leDBk073103ARDecatur Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochem/cals.PRO\MethDB\Decatur Sun AUg 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 5 BC BC 080103 Name: 073103AR-I03 Text : 1 : C8 Acid (PFOA) XC072503-2, 50 ng/h Standard 073103AR-103 Sm (Mn, 2x3) 03-Aug-2003 19:54:17 LC/MS/MS #6 MRM of 4 ChannelsES- 9.13 413 > 369 Area -" ........ , , , .,,. 2.00 ,, J .... 4.00 2:C6 Sulfonate (PFHS) XC072503-2, 50 ng/h Standard 'i .... ,.... 6.00 073103AR-103 Sm (Mn, 2x3) 100-_ _ .... ,,,,_ 8.00 .... , .... 10.00 ,., ..',Time 12.00 8.94 4718- 03-Aug-2003 19:54:17 LC/MS/MS #6 MRM of 4 ChannelsES399 > 80 2.93e4 Area 0' ; .,_, .... 2.00 J ,, ", , , '_',, 4.00 3:C8 Sulfonate (PFOS) XC072503-2, 50 ng/L Standard 073103AR-103 Sm (Mn, 2x3) .... ,"' ', I .... I .... 6.00 8.00 , k.',, . ,',-. ,. ,.'. 10.00 ,Time 12.00 03-Aug-2003 19:54:17 LC/MS/MS #6 MRM of 4 ChannelsES- 9.24 499 > 99 1(o/l _. _ 0-.._--_.. ,-, ,'-:, . , .... 2.00 , .... , .... 4.00 , .... , .... 6.00 29861 , .... , .... , . , -, ", , , . _ 8.00 10.00 1.79e4Area Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:073103AR, Ext.Da_e:07/31/03, Analyet:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals. PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 ll:0&:02 2003 Page 6 Decatur BC BC 080103 Name: 073103AR-I03 Text : 4 : PFOSA XC072503-2, 50 ng/L Standard 073103AR-103 Sm (Mn, 2x3) 03-Aug-2003 19:54:17 LC/MS/MS #E MRM of 4 ChannelsES- 9.89 498 > 78 1(i/1 10303- 5.55e4Area ! 0' .... ,,,, ,, .... ,'..,, _ .... , ,',,. ,".,,. i..", . , .... , .... '_. ,, .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Re_ort _ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\Sam_leDBk073103AR Tue Aug 05 06;59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PR0\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 7 Decatur BC BC 080103 Name: 073103AR-I04 Text : i: C8 Acid (PFOA) XC072503-3, 100 ng/L Standard 073103AR-104 Sm (Mn, 2x3) 03-Aug-2003 20:16:01 LC/MS/MS #6 MRM of 4 Channels ES- 9.15 4'13> 369 0'- ....... , .... 2.00 i .... J .... 4.00 2:C6 Sulfonate (PFHS) XC072503-3, 100 ng/h Standard 073103AR-104 Sm (Mn, 2x3) 1l o0L.._.._ .... L .... 2.00 _. ' ' _ .... 4.00 : C8 Sulfonate (PFOS) XC072503-3, 100 ng/h Standard 073103AR-104 Srn (Mn,2x3) , .... , .... 6.00 L .... i .... 6.00 J .... , _ , 8.00 , . , .... 10.00 ,..-_. ,Time 12.00 03-Aug-2003 20:16:01 LC,%/IS/MS #6 MRM of 4 ChannelsES- 8.98 399 > 80 1 , .... , .... 8.00 , ' ' '--" t .... 10.00 e4a i . , "' _Time 12.00 03-Aug-2003 20:16:01 LC/MS/MS #6 MRM of4 ChannelsES- 9.25 499 > 99 Area 1_1 0'....T:'_,... , . ..,. , .... ',', ,'.. 2.00 4.00 _', , . . , .".. 6.00 , , .... 51001 , , . ,',', .... i , , .--, 8.00 10.00 2.99e4 , _--_ ,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:II:59 2003 Printed: Wed Aug 06 ii:04:02 2003 Page 8 Decatur BC BC 080103 Name: Text: 073103AR-I04 4: PFOSA XC072503-3, I00 n_L Standard 073103AR-104 Sm (Mn, 2x3) 03-Aug-2003 20:16:01 LC/MS/MS #6 MRM of 4 ChannelsES- 9.89 498 > 78 lto/1 20719_ 1.07e5Area i 0 I .... , .... , .... , .... , .... , .... i .... , .... ,'' "' I .... i .... , .... ,Time 2.00 4.00 6.00 8,00 10.00 12.00 V V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Tue Aug 05 06=59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 9 Decatur BC BC 080103 Name: 073103AR-I05 Text : i: C8 Acid (PFOA) XC072503'4, 250 ng/L Standard 073103AR-105 Sm (Mn, 2x3) 03-Aug-2003 20:37:50 LC/MS/MS #6 MRM of 4 ChannelsES- 9.13 413 > 36S 110_ 1285561 7.38e5Area !; ii I .... .-,<--_.. , , .... , .... , . . ' i .... i .... , .... , .... _ .... i .', , . , . . .,,Time 2.00 4.00 6.00 8.00 10.00 12.00 2:C6 Sulfonate (PFHS) XC072503-4, 250 ng/L Standard 073103AR-105 Sm (Mn, 2x3) 03-Aug-2003 20:37:50 LC/MS/MS#6; MRM of 4 ChannelsES-_ 8.98 399 > 80 0 _ .... ", .... , ."_ .-. j .... , .... 2.00 4.00 3:C8 Sulfonate (PFOS) XC072503-4, 250 ng/L Standard 073103AR-105 Sm (Mn, 2x3) ,.... , .... 6.00 , .... , .... 8.00 _ .... 1 .... 10.00 ,.... ,Time 12.00 03-Aug-2003 20:37:51_ LC/MS/MS #_ MRM of 4 Channels ES- 9.25 499 > 99 1i_ ii I .... _'_'.,, .... 2.00 , .... , .... 4.00 i .... , .... 6.00 132851 ,,' ' ' , .... , .... r..'..5 8.00 10.00 7"45e4iArea .... ,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMST\MasslyE_\Fluorochemicals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page i0 Decatur BC BC 080103 Name: 073103AR-105 Text : 4 : PFOSA XC072503-4, 250 ng/L Standard 073103AR-105 Sm (Mn, 2x3) 100_ 03-Aug-2003 20:37:50 LC/MS/MS #6 MRM of 4 ChannelsES- 9.90 498 > 78 48632- 2.52e5 Area i .... i .... , .... r .... i .... , .... _ .... , .... , .... , ....... 2.00 4.00 6.00 8.00 0.00 _'.... _Time 12.00 V V Exygen Research, 3058 Research Drive, State College, PA 16801 I I Quantify Sample Report %_ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PROkSam_leDB\O73103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PROkMethDB\Decatur S_Ln AUg 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 11 Decatur BC BC 080103 Name: 073103AR-I06 Text : i: C8 Acid (PFOA) XC072503-5, 500 ng/L Standard 073103AR-106 Sm (Mn, 2x3) 03-Aug-2003 20:59:39 LC/MS/MS #6 MRM of 4 ChannelsES- 9.13 413 > 369 1'i/1 264862- L 1.51e6Area 1; 0' .... ,._;-_. , , .... _ .'.. ,-.... _ .... , .... _ .... _ ....... _ .... _ .... _Time 2.00 4.00 6.00 8.00 10.00 12.00 _ 2:C6 Sulfonate (PFHS) XC072503-5, 500 ng/L Standard 03-Aug-2003 20:59:39 LC/MS/MS #6 073103AR-106 Sm (Mn, 2x3) 10 J.", .. i .... ,. '... 2.00 , .... i .... 4.00 , .... i .... 6.00 MRM of 4 ChannelsES- 8.98 399 > 80 Area , .... , . , .., .... , .... 8.00 10.00 , .... ,Time 12.00 3:C8 Sulfonate (PFOS) XC072503-5, 500 ng/L Standard 073103AR-106 Sm (Mn, 2x3) 03-Aug-2003 20:59:39 LC/MS/MS #6 MRM of 4 ChannelsES- 9.27 499 > 99 1i1 .... _ .... , .... , ...,.,.... , .... ,.... , .... , ....2897j81.... , .... ,.... ,1T.i6m5e5Area 2.00 4.00 6.00 8.00 10.00 12.00 V Exygen Research, 3058 Research Drive, S_ateCollege, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: _ Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Tus Aug 05 06:59:53 2003 P=\Data\LCMSMS6\Masslyn_\Fluorochemloals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 12 Decatur BC BC 080103 Name : 073103AR-I06 Text : 4 : PFOSA XC072503-5, 500 ng/L Standard 073103AR-106 Sm (Mn, 2x3) 10C 03-Aug-2003 20:59:3_ LC/MS/MS #6 I MRM of 4 Channels ES- I 9.90 104085- 498 > 78I 5.47e5 Area C .... , ,", , , , .... 2.00 ,',,,,, .... ', .... , .... 4.00 6.00 , .... , .... 8.00 ,L ,', ...... 10.00 , .... ,Time 12.00 V Exygen Research, 3058 Research Drive, State / College, PA 16801 Quantify Saz_ple Study No.:L34910, Report Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 13 Decatur BC BC 080103 Naune : 073103AR-I07 Text : i: C8 Acid (PFOA) XC072503-6, 1000 ng/L Standard 073103AR-107 Sm (Mn, 2x3) 03-Aug-2003 21:21:27 LC/MS/MS #6 MRM of 4 ChannelsES- 9.15 413 > 369 1(i/1 5162151 2.96e6Area 1 O ' .... i _-' ' ' _ . ' ' . _ .... _ .... i .... , .... , .... _ .... _ .... I''' '_ .... 1Time 2.00 4.00 6.00 8.00 10.00 12.00 %_ 2:C6 Sulfonate (PFHS) XC072503-6, 1000 ng/L Standard 073103AR-107 Sm (Mn,2x3) 03-Aug-2003 21:21:27 LC/MS/MS #6 MRM of 4 ChannelsES- 8.98 399 > 80 0 _.... I .... ,.... 2.00 _ .... i .... 4.00 3 : C8 Sulfonate (PFOS) XC072503-6, 1000 ng/L Standard 073103AR-107 Sm (Mn, 2x3) L .... , .... 6.00 L .... t .... 8.00 i .... i .... 10.00 , .... ,Time 12.00 03-Aug-2003 21:21:27 LC/MS/MS #6 MRM of4 ChannelsES- 9.27 499 > 99 Area 10=0-_ iI .... _,...., 53617_ 3.12e5 .... ,.... , .... , .... , .... ,.... , .... , .... , .... ,.... t Time V 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 ReSearch D=ive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:073103AR, Ext.Date:07131103, Analyet:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 ii=04:02 2003 Page 14 Decatur BC BC 080103 Name: Text: 073103AR-I07 4: PFOSA XC072503-6, 1000 ng/L Standard 073103AR-107 Sm (Mn, 2x3) 03-Aug-2003 21:21:27 LC/MS/MS #_ MRM of4 ChannelsES- 9.90 498 > 78: O' .... _ .... _.... 2.00 _ .... i .... 4.00 i .... _ .... '6.00 i"' ' '' _ .... 8.00 _ .... _,,, ', _ .... _Time 10.00 12.00 V Zxygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %_ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Da_a\LCMSMS6\Masslynx\Fluoroche_ticals.PRO\Sam_IeDB\073103AR Tue Aug 05 06:59:53 2003 Pz\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04=02 2003 Page 15 Decatur BC BC 080103 Name : 073103AR-I08 Text : 1:C8 Acid (PFOA) L34910-1 Spk C, 5000 ng/L, DF=100 073103AR-108 Sm (Mn,2x3) 03-Aug-2003 21:43:18_ LC/MS/MS #8 I MRM of 4 ChannelsES- I 9.13 413 > 3691 2.96e5-=;I Area C'_.. _-l .,,, .... 2.00 , .... , .... 4.00 2:C6 Sulfonate (PFHS) L34910-1 Spk C, 5000 ng/h, DF=100 073103AR-108 Sm (Mn, 2x3) , .... _, , . . , .... , .... 6.00 8.00 ,' "' '7'' _', .... ,Time 10.00 12.00 03-Aug-2003 21:43:18 LC/MS/MS #6 MRM of4 ChannelsES- 8.98 399 > 80 % - - , , , , .... _ .... 2.00 , .... ,., _ . . , .... , .... 4.00 6.00 3:C8 Sulfonate (PFOS) L34910-I Spk C, 5000 nglL,DF=100 073103AR-108 Sm (Mn, 2x3) i10 _ .... Jl ' [ I' ' _ .... I .... 2.00 , .... 4.00 '' .... , .... 6.00 , . . .', .'... 8.00 , . . , .., .... 10.00 , '.. , i Time 12.00 03-Aug-2003 21:43:1E LC/MS/MS #6 MRM of4 ChannelsES- 9.25 499 99 I e,A I .... ' .... 8.00 ' .... ] ' ' , ", ,-, , ,', Time 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify sample Report %_ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslymx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 16 Decatur BC BC 080103 Name: Text: 073103AR-I08 4: PFOSA L34910-1 Spk C, 5000 ng/L, DF=100 " 073103AR-108 Sm (Mn, 2x3) 03-Aug-2003 21:43:18 LC/MS/MS #6 MRM of 4 ChannelsES- 9.90 496 > 78 11/1 0'T... , .... , .... 2.00 i .... , .... 4.00 , .... , .... 6.00 ,...', , .... 8.00 13039- L , ....... 10.00 6.85e4Area i .... ,Time 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDBk073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6kMasslynxkFluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 17 Decatur BC BC 080103 Name: 073103AR-I09 Text : i: C8 Acid (PFOA) L34910-12 Spk E, 5000 ng/L, DF=100 073103AR-109 Sm (Mn, 2x3) 1% 0 .... C"''' J .... 2.00 _ .... _ .... 4.00 2:C6 Sulfonate (PFHS) L34910-12 Spk E, 5000 ng/L, DF=100 073103AR-109 Sm (Mn, 2x3) 100-_ , .... , .... 6.00 9.13 _ .... r'' ..... 8.00 8.98 % 03-Aug-2003 22:04:5 6 LC/MS/MS #6I MRM of 4 Channels ES- I 413 > 369, 5.53e51 , .... 10.00 ,, _',, ,Time 12.00 i 03-Aug-2003 22:04:5 LC/MS/MS #E MRM of 4 Channels ES399 > 80 Area: 0_', , , . f .... i., ,', r , , ,', _ , , , '. f .... _ , , , _ .... 'r , , , , , ,_-..-.. 2.00 4.00 6.00 8.00 10.00 _ . ,, Time 12.00 3:C8 Sulfonate (PFOS) L34910-12 Spk E,5000 ng/h, DF=100 073103AR-109 Sm (Mn, 2x3) 03-Aug-2003 22:04:56 LC/MS/MS #6 MRM of 4 Channels ES- 9.25 499 > 99 ol oo ooO V 0'... , .... 2.00' ' ' ' ' .... 4.00..'.. ' ...... 6.(30 '''' "-_'-' ' ' ' .......10:00 ' ",-,2, Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\DatakLCMSMS6kMasslynx\Fluorochemlcals.PROkMethDBkDecatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 18 Decatur BC BC 080103 Name: Text: 073103AR-I09 4: PFOSA L34910-12 Spk E, 5000 ng/L, DF=100 073103AR-109 Sm (Mn,2x3) 03-Aug-2003 22:04:5E LC/MS/MS #6 MRM of 4 Channels ES- 9.89 498 > 78 Area i 2.00 4.00 6.00 8.00 10.00 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Saun_le Report _ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last _dified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochem/cals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:kData\LCMSMS6kMasslynxkFluorochem-icals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 19 Decatur BC BC 080103 Na_ne : 073103A_-II0 Text : i: C8 Acid (PFOA) L34910-I 6 Spk F, 5000 n_L, DF=100 073103AR-110 Sm (Mn, 2x3) 10 ,11 01 .... 2.00 [--7 I _ _ _ ' 3 ]'1 _ .... %_f 2:C6 Sulfonate (PFHS) 4.00' .... L34910-I 6 Spk F, 5000 ng/L, DF=100 073103AR-110 Sm (Mn, 2x3) I .... 6.00_ .... 11471 03-Aug-2003 22:26:4_ LC/MSIMS #6[ MRM of 4 Channels ES-_. 6.50e5 I 1i 30 _ * "'.. 8.0J0.... I"'', 10.J00.... , .... 12_.0T0ime 03-Aug-2003LC/MS/MS22:26:48#6 8.96 MRM of 4 Chann3e9ls9 >ES80- Area /100O_ , , , , _ .... L .... 2.00 _ .... _ .... 4.00 3:C8 Sulfona_e (PFOSI L34910-16 Spk F, 5000 ng]L, DF=100 073103AR-110 Sm (Mn, 2x3) 10 "1 _lllJ 2.00 4.00 <'T' ' _ .... 6.00 6.00 t' "' ' _ 1..0..701i _ .... 't .... 8.00 10.00 t'' ''_ _6T.1im38e4 12.00 2240 03-Aug-2003 22:26:40 LC/MS/MS #6) MRM of 4 Channels ES- I 1.26e5 I Areal 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 %qp4 Quantify Sample Study No.:L34910, Report Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103AR 'I"0.8Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochem/cals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 20 Decatur BC BC 080103 Name: Text: 073103AR-II0 4: PFOSA L34910-16 Spk F, 5000 ng/L, DF=100 073103AR-110 Sm (Mn, 2x3) 03-Aug-2003 22:26:40 LC/MS/MS #6 MRM of 4 ChannelsES- 9.90 498 > 78 Area i 1(i/1. 18398- L 9.42e4 0 1 .....,.-,,,,.... ,.... , .... ,.... ,.... ,.... ,....,..,,,,,, _.... ,,, ...,,Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PROkSam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:kData\LCMSMS6\Massly_Ix\Fluorochemicals.PR0kMethDBkDecatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 21 Decatur BC BC 080103 Name: 073103AR-III Text : !: C8 Acid (PFOA) XC072503-1, 25 ng/L Standard i073103AR-111 Sm (Mn, 2x3) 100q ] 9.1: 14631- 03-Aug-2003 22:48:23_ LC/MS/MS #6 MRM of 4 Channels ES- 413> 369i 8.76e4I t_' /_ Area li 0 ....... L-._ , .... j .- . .-_Time 2.00 4.00 6.00 8.00 10.00 12.00 _ 2:C6 Sulfonate (PFHS) XC072503-I, 25 ng/L Standard 03-Aug-2L0C0/M3 S2/2M:S48:#263 073103AR-111 Sm (Mn,2x3) ' 8 98 MRM of 4 Chann3e9l9s>ES8-0 0 __ i 2.00 4.00 3:C8 Sulfonate (PFOS) XC072503-I, 25 n_h Standard 073103AR-111 Sm (Mn, 23) ,_ 6.00 -" - : :: :iTime 8.00 10.00 12.00 03-Aug-2003 22:48:23 LC/MS/MS #6 MRM of 4 ChannelsES- 9.24 499 > 99 1i_,_ .... _ .... _ .... 2.00 _ .... _. 4.00 , _ .... 6.00 t, _,--, , , _.L.._. realL47..3..] _ .... 8.00 10.00 i , , .'. _9/I_.m1i 7ee3 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 22 Decatur BC BC 080103 Name: 073103AK-III Text : 4 : PFOSA XC072503-1,25 ng/L Standard 073103AR-111 Sm (Mn, 2x3) 03-Aug-2003 22:48:23_ LC/MS/MS #6 I MRM of 4 Channels ES- I 9.90 498 > 78J Area _, .. ,--_-, .... , .... 2.00 _ .... _ .... 4.00 , , , . , , .... 6.00 j .... , .... 8.00 , .... , .... 10.00 _-_-_Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sa_ple Report %_ Study No.:L34910, Set No. :073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslyr=x\Fluorochenticals.PRO\SampleDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Massly_ix\Fluorocheaticals.PRO\MethDB\Decatur S%Ln Aug 03 07:11:59 2003 Printed: Wed Aug 06 iI:0_:02 2003 Page 23 Decatur BC BC 080103 Name: 073103AR-I12 Text : I: C8 Acid (PFOA) L34910-1, DF=I 0 073103AR-112 Sm (Mn, 2x3) llv_O_ 03-Aug-2003 23:10:0_ LC/MS/MS #6 I MRM of 4 Channels ES- I 9.13 413 > 369 I 1.26e6] 216041- Area I .... '_" "_...o..o' ....4.o..o..' '""_"_....o. o' ...._.o..o..' ' ..._.o'.o'o' "' ' '_'2:o_e _f_ 2:C6 Su!fonate (PFHS) L34910-1, DF=I 0 073103AR-112 Sm (Mn, 2x3) 03-Aug-2003 23:10:02 LC/MS/MS #6 MRM of 4 Channels ES- 8.98 399 > 80 1to0/1' , ;' i 2.00 3:C8 Sulfonate (PFOS) 534910-1, DF=I 0 073103AR-112 Sm (Mn, 2x3) 100-, J 4.00 r qllil_ 0-' .... _-.... _ .... 2.00 F .... , .... 4.00 , -, , 6.00 _ .... , .... 6.00 _ , ..9..3.81_ : _ ,% 5T.6im1ee4Area 8.00 10.00 12.00 03-Aug-2003 23:10:02 LC/MS/MS #6 MRM of 4 Channels ES- 9.24 499 > 99 161501_ _ .... ,', ,', , , .... _ .... 8.00 10.00 3.57e5 Area , .... i Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report i,_ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:55 2003 P:\Data\LCMSMS6kMasslynx\Fluorocheunlcals.PROkMethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 24 Decatur BC BC 080103 Name: 073103AR-I12 Text : 4 : PFOSA L34910-1, DF=I 0 073103AR-112 Sm (Mn, 2x3) 10_ " 03-Aug-20L0C3/MS23/M:1S0:0#26 . 9.89 MRM of 4 Chann4e9l8s >ES78- 27920- 1,4A3ree5a Ot .... _ .... J' "' '_ .... , .... 2.00 4.00 J .... , .... 6.00 , .... _ .... 8.00 / _'' _] .... 0.00 _ .... ,Time 12.00 t,uM' _J Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha _age 25 Sa/a_le List: Last modified: Method: Last modified: Job Code: P:\Data\LC_SMS6\Masslynx\Fluorochemicals. PRO\Sam_IeDB\073103AR Tue Aug 05 06:59:53 2003 P:\DatakLCMSMS6\Masslynx\Fluorochemicals.PROkMethDBkDecatur Su/1 Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-II3 Text : i: C8 Acid (PFOA) L34910-1 Rep, DF=10 073103AR-113 sm (Mn, 2x3) 03-Aug-2003 23:31:52_ LC/MS/MS #6 I MRM of 4 Channels ES- t 9.13 413 > 369 I ! 1_1 2162681 1.A26reea6 " i 2.00 4.00 6.00 8.00 10.00 12.00 _ 2: C6 Sulfonate (PFHS) L34910-I Rep, DF=10 073103AR-113 Sm (Mn, 2x3) 100 % C; ,-T ._ j 2.00 _ ,J 1 4.00 6.00 03-Aug-2003 23:31:5_ LC/MS/MS #6 MRM of 4 Channels ES- 8.98 10152] i ,", , ...... ._ 8.00 10.00 399 > 801 5.80e4 Are_ ,Time 12.00 3:C8 Sulfonace (PFO5) 534910-1 Rep, DF=10 073103AR-113 Sm (Mn, 2x3) 1007 03-Aug-2003 23:31:52_ LC/MS/MS #6 I MRM of 4 Channels ES- I 9.25 499 > 99 I %t _ll,_.J Area 598881 3.52e5 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sa/n_le Report i_ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/Q3, Analyst:K.Risha Sample List: Last modified: Method: Last modified: job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslyrn(\Fluorochemicals. PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 26 Decatur BC BC 080103 Name: 073103AR-I13 Text : 4 : PFOSA L34910-1 Rep, DF=10 073103AR-113 Sm (Mn,2x3) 03-Aug-2003 23:31:5_ LC/MS/MS #6 MRM of 4 Channels ES- 9.89 498 > 78 Area J 10o_0 .... , .... _ .... 2.00 , .... , .... 4.00 i .... , .... 6.00 _ .', , r _ .... 8.00 27505_ _ .... ,.... 10.00 1.38e5 , .... _Time 12.00 'q,_ Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _pf Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\MethDB\Decatur Su_ Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 27 Decatur BC BC 080103 Name: Text: 073103AR-I14 i: C8 Acid (PFOA) L34910-4, DF=10 073103AR-114 Sm (Mn, 2x3) 03-Aug-2003 23:53:41 LC/MS/MS #6 MRM of 4 Channels ES- 9.13 413 > 369 Area I t_10 _',,, ,'_ , , _ .... 1 .... 1,, , _ .... 1 .... 2.00 4.00 6.00 %_J 2:C6 Sulfonate (PFHS) 534910-4,DF=I0 073103AR-114 Sm (Mn, 2x3) _ .... i 1..3..14151, .... _,, , , i , ,,, i7T.7im4ee5 8.00 10.00 12.00 03-Aug-2003 23:53:41 LC/MS/MS #6 MRM of 4 Channels ES- 8.98 399 > 80 lq!_ 3:C8 Su!fonate 2.00 (PFOS) 4.00 6.00 6122_ 8.00 10.00 3.73e4Area 12.00 L34910-4,DF=I 0 073103AR-114 Sm (Mn, 2x3) 100-_ %tllJ % l 01 .... '_ , , _ .... 2.00 t .... _ .... 4.00 _ .... t .... 6.00 03-Aug-2003LC/MS/MS23:53:41]#_ MRM of 4 Channels ES- / 9.25 499 > 99{ Area J .... , ...4. 492L11.... ,.... 8.00 10.00 '_ .... t2T.5im9ee5 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sa/s_le List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslyn_\Fluorochemicals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6kMasslym-x\Fluorocheraicals.PROkMethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 28 Decatur BC BC 080103 Name: 073103AR-I14 Text : 4 : PFOSA !L34910-4, DF=10 073103AR-114 1 0tv_ Sm (Mn, 2x3) 03-Aug-2003 23:53:41 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 20497- 1.05e5 /l Area i r 01"' f T I [ .... _ '''' ' ' _ .... I .... 2.00 4.00 _ .... _ .... 6.00 _ .... i }'' 8.00 [ I _ ' ' [ .... 10.00 I '1 ' ' " '1 Time 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %U_ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorcchemicals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\DatakLCMSMS6kMasslynx\Fluorochem/cals.PROkMethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 29 Decatur BC BC 080103 Name: 073103AR-I15 Text : i: C8 Acid (PFOA) [L34910-2, DF=I 0 073103AR-115 Sm (Mn, 2x3) I1 9.15 14255 04-Aug-2003 00:15:3_ MRM of 4LCCh/ManSn/MelSs ES#6- /1r 8.29e5 I o_ 2.00 ' 2:C6 Sulfonate L34910-2, DF=I0 (PFHS) 073103AR-115 Sm (Mn, 2x3) 4.00 6.(30 8.;0 8.98 10'00 _ 12'0_ me p 04-Aug-2003 00:15:3G LC/MS/MS #6 MRM of 4 Channels ES399 > 80 107i0 7- ............... -- i---'-'_'_" "; 2.00 ''I _' ' _ ' ' 4.00 3: C8 Sulfonate (PFOS) L34910-2, DF=I 0 073103AR-115 Sm (Mn, 2x3) I_ ' _I ' ' _ 6.00 2.00 4.00 6.00 7036j_ [ '"'' "' i ' ' ;' ,' ' '-' _ '"'--'" 8.00 10.00 4.1A3ere4a ,Time 12.00 04-Aug-2003 00:15:30 LC/MS/MS #6 MRM of 4 Channels ES- 9.27 499 > 99 oI8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %_ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last mmdified: Method: Last mmdified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6kMasslyrm_\Fluorochemicals.PROkMetllDBkDecatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 30 Decatur BC BC 080103 Name: 073103AR-I15 Text : 4 : PFOSA !L34910-2, DF=I 0 073103AR-115 Sm (Mn, 2x3/ 1007 04-Aug-2003 00:15:30 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 _ 16630 498 > 78 8.43e4 Area O''.. _ . : _ .... -._ ,., , , , .... , .... 2.00 4.00 _....,.. ,-...... _ .... ,. ,.., ,..._..... ,, , .... _Time 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: _:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6kMasslyr_xkFluorochemicals.PROkMeth/3B\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 31 Decatur BC BC 080103 Name: 073103AR-I16 Text : : C8 Acid (PFOA) XC072503-2, 50 ng/L Standard 073103AR-116 Sm (Mn, 2x3) 1 0_ ,;o , 0- _", ,_ [ .... 2.00 I .... I .... 4.00 : C6 Sulfonate (PFHS) XC072503-2, 50 ng/L Standard 073103AR-116 Sm (Mn, 2x3) 10 1.... ' .... _ ' I ' 2.00 , .... m .... 4.(30 3:C8 Sulf0nate (PFOS) XC072503-2, 50 n_k Standard 073103AR-116 1 0,_n_ Sm (Mn, 2x3) [ .... '1 .... 6.00 , .... [ .... 6.00 29284- 04-Aug-2003 00:37:1_ LC/MS/MS #6 I MRM of 4 Channels ES- I 1.78e5{ I' 'T_TI '_ '' '_'1 8.00 10.00 4 3 3:i "]''me 12.00 04-Aug-2003 00:37:1 LC/MS/MS #6[ MRM of 4 Channels ES-[ 426 2.73e4/ 86[ oAreaI j ..... _ _ .... 8 _30 r '-, ,. , , _ , _ ._q Time 10'00 12.00 9.2_, 2882- 04-Aug-2003 00:37:1 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1.77e4 %I AA 0, ,,_--_-_-, _, ."_..'_, .... , .... t .... ,.., .-._-i-_--_,. , .... r,-_---_'_-_-_,,.._,Time V 2.00 4.00 6.00 8.00 10.00 Area! 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %_ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemlcals. PROkMethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 32 Decatur BC BC 080103 Name: 073103AR-I16 Text : 4 : PFOSA XC072503-2, 50 ng/L Standard 073103AR-116 Sm (Mn, 2x3) 04-Aug-2003 00:37:19( LC/MS/MS #& MRM of 4 Channels ES- 10890 5.94e4 I 0' .... _ .... _ , _ , , , .... , .... 2.00 4.00 , .... , _ ,-', j .... _ .... 6.00 8.00 _ ....... 0.00 ?,', , , _Time 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify sample Report %_ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochem/cals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 33 Decatur BC BC 080103 Name: 073103AR-I17 Text : I: C8 Acid (PFOA) L34910-6, DF=10 i 073103AR-117 Sm (Mn, 2x3) 100_ 9.13 40498- 04-Aug-2003 00:59:01 LC/MS/MS #6 MRM of 4 Channels ES- I 413 > 369t 2.3A3rea5i 0L-_... /, \. , . j .... 2.00 %_J 2:C6 Sulfonate (PFHS) L34910-6,DF=10 _ .... , .... 4.00 073103AR-117 Sm (Mn, 2x3) 100_ , .... , ., r', .... ,'' '_ 6.00 8.00 '"'',' '"'-' i _' r._Time ! 10.00 12.00 I 8.98 15261 I 04-Aug-2003 00:59:01 LC/MS/MS #6 MRM of 4 ChannelsES399 > 80 9.39e3 Area 2.00 3: C8 Sulfonate (PFOS) L34910-6,DF=I0 073103AR-117 Sm (Mn, 2x3) 4.00 6.00 8.00 10.00 12.00 04-Aug-2003 00:59:01 LC/MS/MS #6 MRM of 4 Channels ES- 9.25 499 > 99 4 100q/ %1 01''' '' _' ' '', 2.00 1..... I .... 'T.... _ .... 4.00 6.00 9224I1 I' _"' ' ,'' ' _'' '' _-'' '-_' 8.00 10.00 5.40e4Area '-'' iTime 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sa/u_le Report I_ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last n%odified: Method: Last modified: Job Code: P:\Data\LCMSMS6kMasslynx\Fluorochemlcals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochem/cals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 34 Decatur BC BC 080103 Name: 073103AR-I17 Text : 4 : PFOSA L34910-6, DF=10 073103AR-117 Sm (Mn, 2x3) 100q 04-Aug-2003 00:59:01 LC/MS/MS #6 MRM of 4 Channels ES- 394.8690- 4918.8>4e748 %1 _i_ 2.00 4.00 6.00 8.00 Area 0.00 12.00 %J Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Saun_le Report _ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last n_odified: Method: Last mmdified: Job Code: P:\Data\LCMSMS6\MasslyrLx\Fluorochermlcals.PRO\SarapleDB\073103AR Tue Aug 05 06:59:53 2003 P:kDatakLCMSMS6iMasslyr_xkFluorocheraicals.PROkMethDBkDecatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 35 Decatur BC BC 080103 Name: 073103AR-I18 Text : i: C8 Acid (PFOA) L34910-6 Rep, DF=10 073103AR-118 Sm (Mn, 2x3) 100- 04-Aug-2003 01:20:44 LC/MS/MS #6 MRM of 4 Channels ES- 9,13 413 > 369 Area C _,, ,)_1 _"',' , , .... 2.00 4.0_0 [ .... .... %_ 2:C6 Sulfonate (PFHS) L34910-6 Rep, DF=I 0 073103AR-118 Sm (Mn, 2x3) 100q _, " , .... 6.00 i .... 3978-"L , 8.00 10.00 J, _, ,'l 2T.3im3ee5 12.00 8.98 1585-_ 04-Aug-2003 01:20:44 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 9.3683 %1 0_ r r [ .... 2.00 _ .... 3: C8 Sulfonate (PFOS) L34910-6 Rep, DF=I0 073103AR-118 Sm (Mn, 2x3) 100-_ i .... 4.00 ] .... _ .... 6.00 _L_ I .... "_ .... J .... '_ .... 8.00 10.00 i rea _ .... i/Ime 12.00 9.27 8484] 04-Aug-2003 01:20:4_ LC/MS/MS #61 MRM of 4 Channels ES499 > 99 5.0284 " I Areal 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sara_le Report _ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\MasslynxkFluorochemlcals.PRO\Sa/npleDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LC_SMS6kMasslyrm_\Fluorochenuicals.PROkMethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 36 Decatur BC BC 080103 Name: 073103AR-I18 Text : 4 : PFOSA L34910-6 Rep, DF=10 073103AR-118 Sm (Mn, 2x3) 100q 04-Aug-2003 01:20:44 LC/MS/MS #6 MRM of 4 Channels ES- 394.8092- 4918.7>6e748 Are_ %1 0 j .... I .... } , T--, 2.00 , ] .... [''' ' ' L .... ' .... 4.00 6.00 ''' '' r'' , _ ........... 8.00 10.00 _Time 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report I_ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslyrux\Fluorochemlcals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\DatakLCMSMS6\Massl3caxkFluorochem/cals.PROkMethDBkDecatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 37 Decatur BC BC 080103 Name: 073103AR-I19 Text : i: C8 Acid (PFOA) L34910-9, DF=10 073103AR-119 Sm (Mn, 2x3) 100-] 9.13 81652- 04-Aug-2003 01:42:36_ r LC/MS/MS #6 I MRM of 4 Channels ES- 413 > 369 4.77e5 Area i 2.00 'ql,,W 2:C6 Sulfonate (PFHS) L34910-9, DF=10 073103AR-119 Sm (Mn, 2x3) 100q % 4.00 .... [ .... J .... 2.00 3:C8 Sulfonate (PFOS) L34910-9, DF=I 0 i .... .... 4.00 073103AR-t19 Sm (Mn, 2x3) 0 _, _ , ',_'_ . , , _ .... 2.00 _ .... i .... 4.00 6.00 i .... , .... 6.00 _ .... _ .... 6.00 8.00 8.98 10.00 12.00 04-Aug-2003 01:42:36 LC/MS/MS #6 MRM of 4 Channels ES- 399 > 80 Area 72 _ .... _ .... _ ,---, , , .... 8.00 10.00 2.31e4 , .... _Time 12.00 04-Aug-2003 01:42:36 LC/MS/MS #6 MRM of 4 ChannelsES- 9.25 499 > 99 i 3e Area i .... _ .... _ .... _ .... _ .... _Time 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Page 38 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslymx\Fluorochemicals. PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\DatakLCMSMS6\Masslynx\Fluorochemlcals.PROkMethDB\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080103 Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-I19 Text : 4 : PFOSA [L34910-9, DF=I 0 073103AR-119 Sm (Mn, 2x3) 04-Aug-2003 01:42:36_ LC/MS/MS #6 i 9 90 MRM of 4 Channels ES- ' Area i 111 8876- 448.447e48 2.00 4.00 6.00 8.00 0.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 _,,_ Quantify Sample Study No.:534910, Report Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMSekMasslyr_x\Fluorochealicals. PROkMethDBkDecatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 39 Decatur BC BC 080103 Name: 073103AR-120 Text - i: C8 Acid (PFOA) 534910-7, DF=10 073103AR-120 Sm (Mn, 2x3) lq0_ 04-Aug-2003 02:04:23 LC/MS/MS #6 MRM of 4 Channels ES- 9.13 413 > 369 112700- 6.62e5 Area i 0I ',/_'. ' ' _ '.' _ .... _ .... _ .... "' . ' , .... ....... 2.00 4.00 6.00 8.00 _ 2:C6 Sulfonate (PFHS) L34910-7, DF=10 073103AR-120 Sm (Mn, 2x3) 8.97 'r .... ','... ,Time 10.00 12.00 04-Aug-2003 02:04:23 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1_1 0 I' ' ''_--_'-'_' ' '-_ I ] 2.00 ' r I .... 3: C8 Sulfonate (PFOS) L34910-7, DF=10 t " ''' 4.00 ' I' ' r _ .... 6.00 073103AR-120 Sm (Mn, 2x3) % I .... 6025_ I .... ] .... I .... 8.00 10.00 l .... ,3T.i6Am6ree8a4 12.00 04-Aug-2003 02:04:23 LC/MS/MS #6 MRM of 4 Channels ES- 9.25 499 > 99 Area 10! 1 0 _ .... qllt_ll' _ r' ', .... 2.00 _ .... , .... 4.00 , .... , .... 6.00 292841 _ .... , .... , .... _ .... 8.00 10.00 1.69e5 , .... ,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 I Quantify sample Report _ Study No.:L34910, Set No.:073103A_, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslyru_\Fluorochemicals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorocheunicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 40 Decatur BC BC 080103 Name: 073103AR-120 Text : 4 : PFOSA L34910-7, DF=10 073103AR-120Sm (Mn, 2x3) J10.0'_- 1 _.oo 4.o0 _.oo 04-Aug-2003 02:04:23_ LC/MS/MS #6 I MRM of 4 Channels ES-I 9.89 11595- 496 > 78 5.A91reea4i_ 1 _.oo lO.OO ,_.oo Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %_ Study No.:L3_910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last n_Ddified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur Sun Aug 03 07:11:59 2005 Printed: Wed Aug 06 11:04:02 2003 Page 41 Decatur BC BC 080103 Name: 073103AR-121 Text : i: C8 Acid (PFOA) XC072503-3, 100 ng/L Standard 073103AR-121 Sm (Mn,2x3) 10C_j i 9.15 55667- 04-Aug-2003LC/MS/MS02:26:03#6 MRM of 4 ChannelsES413 > 36! 3.27e! Are_ .... , .... , .... , .... 2.00 4.00 2:C6 Sulfonate (9FHS) XC072503-3, 100 ng/L Standard 073103AR-121Sm (Mn, 2x3) ,o1o 0 _ J .... J .... 2.00 _ .... _ .... 4.00 3:C8 Sulfonate (PFOS) XC072503-3, 100 ng]L Standard 073103AR-121 Sm (Mn, 2x3) , .... ,.., 6.00 _ ' } ;' ' , .... 6.00 E .... _ ...... 8.00 L ' ,,' ' '_-_'' 10.00 ,-'iTime 12.00 8.98 9486 04-Aug-2003 02:26:03 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 5.49e4 Area , .... j ' I ; 8.00 J .... 10.00 _', ,-,,Time 12.00 04-Aug-2003 02:26:03_ LC/MS/MS #6 t MRM of 4 Channels ES- 9.27 499 > 99 lly10 t .... q-f%'',' , .... ,', ,., , .... ,,, '_' , .... I .... T .... 600,4L' ' ,, .... _ .... 3iT"iA4m9ree8a4 V 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify sample Report %_ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sara_le List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorocheaticals.PR0\SampleDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals. Sun Aug 03 07:11:59 2003 PRO\MethDB\Decatur Printed: Wed Aug 06 11:04:02 2003 Page 42 Decatur BC BC 080103 Na/ne : 073103AR-121 Text : 4 : PFOSA XC072503-3, 100 ng/L Standard 073103AR-121 Sm (Mn, 2x3) ool 1j_n,r,_, - 0 _ ' ' ' .` ' .... [' J'''''' _ .... 2.00 ' .... 4.00 ', .... _ .... 6.00 _ .... ] .... 8.00 04-Aug-2003 02:26:03 LC/MS/MS #6 MRM of 4 Channels E5- 9.90 _ 498 > 78 21221 1.12e5 Area _ ........ J i. 0.00 _Time ' .... 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last z_odified: Method: Last _dified: Job Code: _:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Tue Aug 05 06:59:55 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 43 Decatur BC BC 080103 Name: 073 I03AR-122 Text : i: C8 Acid (PFOA) L34910-12, OF=20 /073103AR-122 Sm (Mn, 2x3) 1 00q, % 0" .... _ ] '' j .... 2.00 J .... ' .... 4.00 _ 2:C6 Sulfonate (PFHS) L34910-12, DF=20 073103AR-122 Sm (Mn, 2x3) _ .... _ .... 6.00 04-Aug-20L0C3/MS0/2M:4S7:4#76 MRM of 4 Channels ES- 9.13 413 > 369 1 3089111 1.81e6 I i , _ .... 8.00 Area .... .... ,.- ,Time 10.00 12.00 04-Aug-2003 02:47:47 LC/MS/MS #6 MRM of 4 Channels ES- 2616 1.54e5 2.00 4.00 6.00 8.00 _ 10,.00 . _ 12,.0T0Aimreea _ 0 I r , _ _ , , , _ I .... I .... [ .... I .... I .... _' ' ' II] II i ' '[ _ ' ] ' II 3:C8 Sulfonate (PFOS) L34910-12, DF=20 073103AR-122 Sm (Mn, 2x3) 04-Aug-2003 02:47:4_ LC/MS/MS #6J MRM of 4 Channels ES- 9.25 499 > 99 1(/!_,_ 0! j .... [ 2.00 , .... _ .... 4.00 [ .... [ I f r' ' j .... 6.00 644991 [ .... I .... 8.00 ' .... 10.00 3.81e5Area ' .... ,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sau_le Report _ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Lash modified: Job Code: P:\Data\L_qSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\MasslynxkFluorochemlcals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 44 Decatur BC BC 080103 Na_e: 073103AR-122 Text : 4 : PFOSA L34910-12, DF=20 073103AR-122 Sm (Mn, 2x3) 100 %- 04-Aug-2003 02:47:4 i LC/MS/MS #6 I MRM of 4 Channels ES-L 9.88 24495- 498 > 78 1.25e5 Area G .... r .... _ .... 2.00 _ .... t "' 4.00 , , i .... .... 6.00 _ .... / .... 8.00 L ....... 0.00 i .... _Time 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %_ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochamlcals.PRO\MethDBkDecatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 45 Decatur BC BC 080103 Name: 073103AR-123 Text : i: C8 Acid (PFOA) L34910-12 Rep, DF=20 073103AR-123 Sm (Mn, 2x3) 1 yo 9.13 315651 04-Aug-20L0C3/MS0/3M:0S9:2#_6 MRM of 4 Channels ES- 1.84e6I .... I--', , , _ .... 2.00 %_f 2:C5 Sulfonate (PFHS) L34910-I2 Rep, DF=20 _ .... , .... 4.00 073103AR-123 Sm (Mn, 2x3) 01 0_ .... ,' '" ' ' , .... 2.00 3:C8 Sulfonate (PFOS) L34910-12 Rep, DF=20 , .... _ .... 4.00 073103AR-123 Sm (Mn, 2x3) _ .... _,-,,, 6.00 h .... d .... 6.00 _,, ,'-: _ .... 8.00 _ .... _ .... 10.00 , .... _Time 12.00 04-Aug-2003 03:09:25 LC/MS/MS #6 MRM of 4 Channels ES- 8.98 399 > 80 Area , .... _, ',',, j .... , .... 8.00 10.00 _ .... _Time 12.00 04-Aug-2003 03:09:25 LC/MS/MS #6 MRM of 4 Channels ES- 9.25 499 > 99 1_1 64047_ 3.75eSArea 0: .... i .... I .... _ .... _ .... I .... _ .... E.... _ .... _ .... I .... I .... _Time V 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample ReDort %_ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDBk073103AR Tue Aug 05 06:59:53 2003 P:kData\LC_SMS6kMasslynxkFluorochealicals.PROkMethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 46 Decatur BC BC 080103 Name: 073103AR-123 Text : 4 : PFOSA L34910-12 Rep, DF=20 073103AR-123 Sm (Mn,2x3) 100- %_ 04-Aug-2003 03:09:2_ LC/MS/MS #61 MRM of 4 Channels ES-t 9.89 498 > 78! 23261- 1.19e5 Area 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %_ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last m_dified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochem/cals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 47 Decatur BC BC 080103 Name: 073103AR-124 Text : i: C8 Acid L34910-15, (PFOA) DF=20 073103AR-124 Sm (Mn, 2x3) 04-Aug-2003 03:31:0S_ LC/MS/MS #61 MRM of 4 Channels ES- 9.14 413 > 369 :0" .... _->, , , _ .... 2.00 , .... _ .... 4.00 '_ .... d .... 6.00 ,',,,, ,-', ...... 8.00 i _ .... 10.00 ea l _ .... ,Time 12.00 _j 2:C6 Sulfonate (?FHS) IL34910-15, DF=20 04-Aug-2003 03:31:09 LC/MS/MS #6 073103AR-124 Sm (Mn, 2x3) MRM of 4 Channels ES- 8.98 399 > 80 0' .... _ .... I r.. , , i .... _ .... 2.00 4.00 J .... _ .... 6.00 41 1 .... _ .... 8.00 _ .... ,.... 10.00 6Area _ .-,,, ,Time 12.00 3:C8 Sulfonate (PFOS) L34910-15,DF=20 073103AR-124 Sm (Mn,2x3) 04-Aug-2003 03:31:09 LC/MS/MS #6 MRM of 4 ChannelsES- 9.27 499 > 99 Area 0 t .... , .... t .... _ .... , .... L.... _, , , , _ .... _ .... i ,,, , .... _ .... ,Time _W 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %_j Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha San_le List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslyru(kFluorochemicals.PRO\SampleDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochem/cals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 48 Decatur BC BC 080103 Name: Text: 073103AR-124 4: PFOSA L34910-15, DF=20 t073103AR-124 Sm (Mn, 2x3) 04-Aug-200L3C/MS0/3M:S31:09#_ MRM of 4 Channels ES_ 1110 _ 9.90 498 > 7_ ! %,,,,,# Area .... J .... , .... _ .... , .... _ .... _ .... _ .... i .... , .... , _-,, _ .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last m_dified: Method: Last I_odified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals. PR0\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 49 Decatur BC BC 080103 Name: 073103AR-125 Text : I: CS Acid (PFOA) L34910-I 3, DF=20 073103AR-125 Sm (Mn, 2x3) 10C 04-Aug-2003 03:52:55 LC/MS/MS #6 MRM of 4 Channels ES- 9.13 413 > 369 354730- 2.09e6 Area ' C .... ,'g_'' ' '_ .... 2.00 _w_' 2:C6 Sulfonate (PFHS) , .... _ .... 4.00 _ .... , .... 6.00 ,L , .... _ ....... 8.00 I .... 10.00 , .... ,Time 12.00 L34910-13, DF=20 /073103AR-125 Sm (Mn, 2x3) 04-Aug-200L3C/MS0/3M:S52:5#56 MRM of 4 Channels ES- 8.98 399 > 80 1_1 3:C8 Sulfonate 2.00 (905) 4.00 6.00 306731 8.00 10.00 1.82e5Area 12.00 L34910-13, DF=20 LC/MS/MS #6 04-Aug-2003 03:52:55 t073103AR-125 Sm (Mn, 2x3) 9.25 MRM of 4 Chann4e9ls9 >ES99- 100_ t o,j I77839-_ 4.48e5 Area 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report V Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\DatakLCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PROkMethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 50 Decatur BC BC 080103 Name: 073103AR-125 Text : 4 : PFOSA L34910-13,DF=20 073103AR-125 Sm (Mn, 2x3) 1OO_ 04-Aug-2003 03:52:55 LC/MS/MS #6 MRM of 4 Channels ES- 295.79306- 4918.2>97e85I Area [ .... j .... 2.00 [ r r t'" ,--] .... 4.00 ' i i-- f , , [ .... 6.00 ] .... ] .... 8.00 i , , ,J .... 0.00 I ' " "' I Time 12.00 'IV Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last r&odified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 51 Decatur BC BC 080103 Name: 073103AR-126 Text : I: C8 Acid (PFOA) XC072503-4, 250 ng/L Standard 073103AR-126 Sm (Mn, 2x3) 04-Aug-2003 04:14:42_ LC/MS/MS #6 t MRM of 4 Channels ES- I 9.13 413 > 36!9 Area 0 _ .... '_'_' ' ' _ .... 2.00 I .... J .... 4.00 %mS 2:C6 Sulfonate (?HS) XC072503-4, 250 ng/L Standard 073103AR-126 Sm (Mn, 2x3) J .... I .... 6.00 i .... i .... 8.00 I ,,' J .... 10.00 , .... ,Time 12.00 04-Aug-2003 04:14:42_ LC/MS/MS #_ MRM of 4 Channels ES- I 8.96 399 > 80I 01 .... _ .... .... 2.00 ,.... _ .... 4.00 3:C8 Sulfonate (PFOS) XC072503-4, 250 ng/L Standard 073103AR-126 Sm (Mn, 2x3) 10 Ii ' %_ 2.00 4.00 J .... .... 6.00 6.00 j .... r-, .... 8.00 .... 10,00 .... _Time 12.00 04-Aug-2003 04:14:42 LC/MS/MS #6 I MRM of 4 Channels ES- I 1328 7.65e4 Area 9.2 9 8.00 10.00 499,991 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Massllrnx\Fluorochemicals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\DatakLCMSMS6kMasslynxkFluorochemicals.PROkMethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 52 Decatur BC BC 080103 Name: 073103AR-126 Text : 4 : PFOSA XC072503-4, 250 ngJt Standard 073103AR-126 Sm (Mn,2x3) 100-t 04-Aug-2003 04:14:42_ LC/MS/MS#6I MRM of 4 Channels ES-! 9.92 498 > 78 49195- 2.56e5 Area o_t--'1' ] f J '" ' ' ' , ' ]' ] ] ] .... 2.00 ] .... 4.00 _ .... _ .... 6.00 '] ' ' , _, , , , _ ....... 8.00 '10.00 _ .... _Time 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set NO.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslymx\Fluorochemicals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochem/cals. PRO\MethDB\Decatur Sun AUg 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 53 Decatur BC BC 080103 Name: 073103AR-127 Text : i: C8 Acid L34910-16, (PFOA) DF=100 073103AR-127 Sm (Mn, 2x3) 04-Aug-2003 04:36:3C LC/1VIS/MS #6 MRM of 4 Channels ES- 9.13 413 > 369 100].. 825151 4.7A3ree_= '. 0_, , ,'F-.... , .... _. ,-., , _ .... _ , , , _,,,-, , , , ,-_ .... _,, _--_-.... _ .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 %_ 2:C6 Sulfonate (PFHS) L34910-16,DF=100 073103AR-127 Sm (Mn, 2x3) 10 04-Aug-2003 04:36:3 LC/MS/MS #_ MRM of 4 Channels ES- 687 3.82e4 Area i/l ,, ," , T , ] 2.00 3:C8 Sulfonate (PFOS) IL34910-I6,DF=100 073103AR-127 Sm (Mn,2x3) ', ," 4.00 6.00 8.9__ 8.00 t 10.00 399 > 80 12.00 04-Aug-2003 04:36:30 LC/MS/MS #6 MRM of 4 Channels ES- 9.27 499 > 99 li0_Fo_] 01 .... _, ,',,, .... j .... _ .... , 2.00 4.00 _ .... 6.00 170941 ,.... , ,. ,", , .... _ .... 8.00 10.00 9.90e4Area _ .... _Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Re_ort %_ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Tue Aug 05 06:59:53 2003 P:\Dat_iLC_SMS6\Masslyr_x\Fluorochemicals.PROiMetb-DB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 I1:04:02 2003 Page 54 Decatur BC BC 080103 Name: 073103AR-127 Text : 4 : PFOSA L34910-16, DF=100 073103AR-127 Sm (Mn,2x3) I100 %- 04-Aug-20L0C3/MS04/M:3S6:3#06 MRM of 4 Channels ES- 67181 9.89 3.52e4 498A>r7e8a _-_-, r-_"_"_,,, , , ',-_ _ , __ Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %_ Study No.:534910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last m_dified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Tue Aug 05 06:59:55 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 55 Decatur BC BC 080103 Name: 073103AR-128 Text : i: C8 Acid (PFOA) 534910-16 Rep, DF=100 073103AR-128 Sm (Mn, 2x3) 100_ %t] 9.13 83658- 04-Aug-2003 04:58:16 LC/MS/MS #6 MRM of 4 Channels ES413 > 369 4.68e5 Area ] 2.00 _ 2:C6 Sulfonate (PFHS) L34910-16 Rep, DF=100 073103AR-128 Sm (Mn, 2x3) 4.00 6.00 8.00 6261 10.00 12.00 04-Aug-2003 04:58:16 LC/MS/MS #6 MRM of 4 Channels ES- 3.59e4 Area 0' .... , .... , ' "', _ .... _ .... 2.00 4.00 3:C8 Sulfona_e (PFOS) L34910-16 Rep, DF=100 073103AR-128 Sm (Mn, 2x3) i' "" ' ' , .... 6.00 i .... , , , , _ .... q-,_,,,, 8.00 10.00 ', , _:Time 12.00 04-Aug-2003 04:58:16 LC/MS/MS #6 MRM of 4 Channels ES- 9.27 499 > 99 01% 0_ .... _, ,-, , _ , , , r .... , .... "'_ .... , .... 2.00 4.00 6.00 1726 _ .... r .... _ .... _ .... 8.00 10.00 9'56e4iArem J .... _Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sa_le Study No.:L34910, Report Set No.:073103AR, Ext.Date:07/3!/03, Analyst:K.Risha Sample List: Last mmdified: Method: Last mmdified: job Code: P:\Data\LCMSMS6\Masslynx\F1uorochemicals.PRO\San_pleDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochem/cals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 56 Decatur BC BC 080103 Name: 073103AR-128 Text : 4 : PFOSA L34910-16 Rep, DF=100 !073103AR-128 Sm (Mn, 2x3) 04-Aug-20L0C3/MS04/M:5S8:1#6 MRM of 4 Channels ES- 9.92 498 > 78 J ,-r , , _ .... _ .... "_ ,',, , ,-, , , _ ,--_, , _', ,,'' _'' 'r-' _ .... 2.00 4.00 6.00 8.00 T _ ' ' ' E' ' '= _" ' '' _Time 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 %_mf Quantify Sample Study No.:534910, Report Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sau_le List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 57 Decatur BC BC 080103 Name: 073103AR-129 Text : i: C8 Acid (PFOA) 534910-19, DF=100 '073103AR- 129 Sm (Mn, 2x3) ; 04-Aug-2003LC/MS/MS05:20:01#E MRM of 4 Channels ES- 9.13 413 > 36g Area i 1i/1 75424 i 4.39e5 . 0 ' .... -_-' r ' ' ] ] .... ] .... l .... j .... j .... [' ' ' ' ' , ' '--_'' _ .... , ' ''_ ' j "' ' ' j Time 2.00 4.00 6.00 8.00 10.00 12.00 %_f 2:C6 Sulfonate (PFHS) L34910-I 9, DF=100 073103AR-129 Sm (Mn, 2x3) il0-_ , , L' , i _ 2.00 3:C8 Sulfonate (PFOS) 534910-19, DF=100 073103AR-129 Srn (Mn, 2x3) ' ' J ' ' ' ,'' __q-- 4.00 6.00 04-Aug-2003 05:20:01 LC/MS/MS #6 MRM of 4 Channels ES- 8.96 399 > 80: 611 7-'. ' . _. , r . j .... _ Time 8.00 10.00 12.00 I 04-Aug-2003 05:20:01] LC/MS/MS #6 MRM of 4 Channels ES-! 9,25 499 > 99 100/_iJ 168611 0 ! .... r .... _ , , , r .... F,',,, J .... , ,, , , _ .... _ .... _ .... ,',,,, 9'gA6reaa _ .... ,Time V 2.00 4.00 6.00 8.00 10.00 12.00 I Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify sample Report _ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last mmdified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochem-icals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochera/cals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 ii:04:02 2003 Page 58 Decatur BC BC 080103 Name: 075103AR-129 Text : 4 : PFOSA L34910-19, DF=100 073103AR-129 Sm (Mn,2x3) 1,_,-, u_ 04-Aug-2003 05:20:01 LC/MS/MS #6 MRM of 4 Channels ES- 9.89 498 > 78 65061 3.33e4Area 0_ _,_ '----r-r-T' i .... 2.00 I' "' _ 4.00 6.00 I ........ 8.00 J ' ' ' r ...... 10.00 j Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 I I Quantify Sample Report _ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last mmdified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslyr_x\Fluorochamicals.PRO\SampleDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Massly_x\Fluorocheunicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 ii:04:02 2003 Page 59 Decatur BC BC 080103 Name: 073103AR-130 Text : i: C8 Acid (PFOA) 534910-17, DF=100 073103AR-130 Sm (Mn, 2x3) 04-Aug-2003 05:41:49_ LC/MS/MS #6 I MRM of 4 Channels ES- I 9.13 413 > 369[ 4.61e51 1101 785361 Area : 2.OO 4.LOu ";''''''6.00 .... ' .... 8.00..'.. '''' l'0.,0,,u.,-, ..... , 1,2T,^il.j.u _ 2:C6 Sulfonate (PFHS) L34910-17, DF=100 073103AR-130 Sm (Mn, 2x3) 04-Aug-2003 05:41:49 LC/MS/MS #6, MRM of 4 ChannelsES- 8.98 399 > 80 f 11/L _ : . _, _ .... 2.00 3:C8 Sulfonate (PFOS) 534910-I7, DF=100 _ .... , .... 4.00 073103AR-130 Sm (Mn, 2x3) 10(_ _ .... _ .... 6.00 _ .... _ ..6..01 _ .... _,, .-_ _ .... "_3T.A5im5re8ea4 8.00 10.00 12.00 196.122! 3- 04-Aug-2003 05:41:49] ! LC/MS/MS #6 i MRM of 4 Channels ES- 4999.4>39e941 AreaJ ,1,_j, Jl OF.. ' ' ' J .... I .... 2.00 I .... I .... 4.00 J .... f .... 6.00 I .... J" ...... 8.00 I ' '"' ' , .... t Time 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _! Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha San_le List: Last modified: Method: Last modified: Job Code: P:kData\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6kMasslynxkFluorochemicals.PROkMethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 60 Decatur BC BC 080103 Name: 073103AR-13Q Text : 4 : PFOSA L34910-17, DF=100 073103AR-130 Sm (Mn, 2x3) 4 10_o0__ 2.00 4.00 6.00 04-Aug-2003 05:41:4.c LC/MS/MS #6 MRM of 4 Channels ES- 9.89 498 > 78 5831L 8.00 10.00 Area I 3.0184 ' 12.00 %,,# Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report I_ Study No. :L34910, Set No. :073103AR, Ext.Date:07/31/03, A/lalyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\DatakLCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:iData\LCMSMS6iMasslynxkFluorochemicals.PRO\MethDBkDecatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 61 Decatur BC BC 080103 Name: 073103AR-131 Text : i: C8 Acid (PFOA) XC072503-5, 500 ng/L Standard 073103AR-131 Sm (Mn, 2x3) 100q 9.15 2719061 04-Aug-2003 06:03:36 LC/MS/MS #6 MRM of 4 Channels ES413 > 369 1.53e6 1 ! 01,', , , j_J-'_, , _ .... 2.00 j .... _ .... 4.00 _ .... _ .... 6.00 _ .... _ .... 8.00 Area _ .... _'", , , , j', , ,", _Time 10.00 12.00 _ 2: C6 Sulfonate (PFHS) XC072503-5, 500 ng/L Standard 073103AR-131 Sm (Mn, 2x3) 04-Aug-2003 06:03:36 LC/MS/MS #6 MRM of 4 Channels ES- 8.96 399 > 80 10/(}_]=! 2.00 4.00 3:C8 Sulfonate (POS) ,XC072503-5, 500 ng/L Standard 073103AR-131 Sm (Mn, 2x3) 6.00 454961 8.00 10.00 2.6A1rea5 12.00 04-Aug-2003 06:03:36 LC/MS/MS #6 MRM of 4 Channels ES- 9.27 499 > 99 Area _J 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 12.00 Quantify sample Report %_ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last m_dified: Method: Last n_odified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorocheznicals.PRO\SampleDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslyrn_\Fluorochamicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 62 Decatur BC BC 080103 Name: 073103AR-131 Text : 4 : PFOSA XC072503-5, 500 ng/L Standard '073103AR-131 Sm (Mn, 2x3) 100_ 04-Aug-2003 06:03:36 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 %i__ 0-I .... I .... _ ' '-' ' I ' "'--"i .... 2.00 4.00 I .... l"' 6.00 ' I .... i .... 8.00 1022921 _ ''' ' i .... 10.00 5.2A2ree5a I .... i Time 12.00 r V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %_ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha San_le List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 63 Decatur BC BC 080103 Naune : 073103AR-132 Text : i: C8 Acid (PFOA) L34910-16, DF=20 073103AR-132 Sm (Mn, 2x3) 100_ . 9.13 380900- 04-Aug-2003 06:25:24 LC/MS/MS #6 MRM of 4 Channels ES- 413 > 369 2.20e6 %l Area i 4 4 L 0J .... 'r-,, _ .', .... 2.00 , .... r .... 4.00 i .... i .... 6.00 J .... , .... 8.00 k, . . , .... 10.00 , .... ,Time 12.00 _I_ 2:C6 Sulfonate (PFHS) L34910-16, DF=20 073103AR-132 Sm (Mn, 2x3) 04-Aug-2003 06:25:24 LC/MS/MS #6 MRM of 4 Channels ES- 8.96 399 > 80 I100_ 330041 1.86e5Area - 2.00 4.00 6.00 8.00 10.00 12.00 : C8 Sulfonate (PFOS) L34910-16, DF=20 073103AR-132 Sm (Mn, 2x3) 04-Aug-2003 06:25:24 LC/MS/MS #6 MRM of 4 Channels ES- 9.26 499 > 99 ; 1i_ '_''' [ _ ' ' ' , . .'-' _ .... ;.... ,''', 818621 4.68e5Are_ i .... _ ' ' ' ' ,",'', .... _ "'' 'I .... _Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:kData\LCMSMS6kMasslynx\Fluorochemicals.PRO\San_leDBk073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Name: 073103AR-132 Text : 4 : PFOSA Page 64 Decatur BC BC 080103 L34910-16, DF=20 073103AR-132 Sm (Mn, 2x3) /l_r, 04-Aug-2003 06:25:2_ LC/MS/MS #6[ MRM of 4 Channels ES- 9.89 32659_ 498> 78 1.6485 / i1 i Areal 2.00 4.00 6.00 8.00 10.00 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample ReDort _ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:kData\LCMSMS6kMasslynxkFluorochemicals.PROkMetb_DBkDecatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 ii:04:02 2003 Page 65 Decatur BC BC 080103 Name: 073103AR-133 Text : i: C8 Acid L34910-16 (PFOA) Rep, DF=20 073103AR-133 Sm (Mn, 2x3) 10C % 9.12 391789- 04-Aug-2003 06:47:2f, LC/MS/MS #6 MRM of 4 Channels ES413 > 36 2.26e6 Area C .... i_', ,, _ .... 2.00 %,.J 2:C6 Sulfonate (PFHS) _ .... i ' ' ' _ '" ' , .... 4.00 6.00 f .... _ ....... 8.00 _ .... 10.00 _ ' ' , ,Time 12.00 L34910-I 6 Rep, DF=20 073103AR-133 Sm (Mn, 2x3) LC/MS/MS #6 04-Aug-2003 06:47:22 8.97 MRM of 4 Chann3e9ls9 E>S8-0 Area -t/100_1 30633_ 1.81e5 0 _ .... I .... I '-'' ' i .... , .... I , f .... j .... , .... j .... , .... ,-,','., _Time 2.00 4.00 6.00 8.00 10.00 12.00 3:C8 r Sulfonate (PFOS) L34910-I 6 Rep, DF=20 073103AR-133 Sm (Mn, 2x3) 04-Aug-2003LCS/0M6S:/4M7:2_#6 9.25 MRM of 4 Chann4e9ls9 >ES9-9 100q%1 0 / .... _ .... .... 2.00 _ .... , .... 4.00 ,-, , , _ .... 6.00 8426311 , , .',, _ .... , .... _ .... 8.00 10,00 4.80e51Area _ .... _Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sau_le Report _ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method : Last modified: Job Code : P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P : \Data\LCMSMS6 \Masslynx\Fluorocham/cals. PROkMethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 66 Decatur BC BC 080103 Name: 073103AR-133 Text : 4 : PFOSA IL34910-16 Rep, DF:20 073103AR-133 Sm (Mn, 2x3) 1 04-Aug-2003 06:47:22_ LC/MS/MS #6 I MRM of 4 Channels ES- I 3191 1.61e5' Areal p 0-_''' ' _ .... b, ,",, J .... , , , ," _ , ., r .... 2.00 4.00 6.00 _ .... _ ....... , 8.00 _ , , , , _ r , , , ,Time 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _# Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorocheunicals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 67 Decatur BC BC 080103 Name: 073103AR-134 Text : : C8 Acid L34910-19, (PFOA) DF=20 073103AF_-134Sm (Mn, 2x3) 100] i 04-Aug-2003 07:09:05_ 9.13 364595- MRM of 4LCC/hMaSnn/MelSs E#S.6! 413 > 369 2.02e6 Area i .... _--,.,,,, .... 2.00 : C6 Sulfonate (PFHS] L34910-I9,DF=20 p .... ., .... 4.00 073103AR-134 Sm (Mn, 2x3) _ .... _ .... 6.00 _ .... _ ....... 8.00 8.96 , .... 10.00 _ .... ,Time 12.00 04-Aug-2003 07:09:05 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 Area 2.00 3:C8 Sulfonate (PFOS) L34910-19, DF=20 073103AR-134 Sm (Mn, 2x3) 1 4.00 6.00 0-j .... , .... r , , , _ .... , , , , _d 2.00 4.00 6.00 8.00 10.00 12.00 9.2__ 82201 04-Aug-2003 07:09:05_ LC/MS/MS #6 r MRM of 4 Channels ES- I 4.64e5 l 4 r2Z k , _ .... _ .... ,Timer 8.00 10.00 12.00 ] Exygen Research, 3058 Research Drive, State College, PA 16801 I ' Quantify Sample Report _ Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last mmdified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslyru_\Fluorochem/cals.PRO\San_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\MasslyrnckFluorochemicals.PRO\MethDBkDecatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 68 Decatur BC BC 080103 Name: 073103AR-134 Text : 4 : PFOSA L34910-19, DF=20 073103AR-134 Sm (Mn, 2x3) 04-Aug-2003 07:09:05_ LC/MS/MS #6! 9.90 MRM of 4 Channels ES- 100_ 32869- 4918.6>87e85I1 Areal "] 2.00 4.00 6.00 8.00 10.00 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify sample Study No.:L34910, Report Set No.:073105AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Tue Aug 05 06:59:53 2005 P:\Data\LCMSMS6\Masslynx\Fluorochemicals. PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 69 Decatur BC BC 080103 Name: 073103AR-135 Text : i: C8 Acid (PFOA) L34910-I 7, DF=20 073103AR-135 Sm (Mn, 2x3) ' 04-Aug-2003LCIMS/MS07:30:42#6 MRM of 4 Channels ES- 9.11 413 > 369 Area i 100-_ O_ .... ",-_ ' ' ' , .... 2.00 r .... J .... 4.00 f .... J .... 6.00 3628981 + ,, , , ,-, , , , , .... + .... 8.00 10.00 2.08e6 j .... ,Time 12.00 _ 2: C6 Sulfonate {PFHS) L34910-17, DF=20 073103AR-135 Sm (Mn, 2x3) 1 0_, ,/o 2866 04-Aug-2003 07:30:42_ LC/MS/MS #6 i MRM of 4 Channels ES- 1.69e51 0 .... i .... _ i . . . _ .... _ .... 2.00 4.00 3:C8 Sulfonai:::e (PFOS) L34910-17, DF=20 073103AR-135 Sm (Mn, 2x3) F .... i .... 6.00 _ .,. _ .... 8.00 i, _', ,', .... 10.00 J _ .... ,Timel 12.00 04-Aug-2003 07:30:42_ ! LC/MS/MS#6i MRM of 4 Channels ES- I 9.25 499 > 99 I lql 0 1 .... _ .... _ .... 2.00 + . . . , .... 4.00 _, '' ' E .... 6.00 796981 , .... + .... _ .... ,,. 8.00 10.00 + .... 4.4A4r8e5a '_Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:073103AK, Ext.Date:07/31/03, Analyst:K.Risha Samp!e List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\073103AR Tue Aug 05 06:59:53 2003 P:\DatakLCl_SMS6\Masslyr_\Fluorocheraicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 70 Decatur BC BC 080103 Name: 073103AR-135 Text : 4 : PFOSA ]L34910-17,DF=20 073103AR-135 Sm (Mn, 2x3) 04-Aug-2003 07:30:42 LC/MSIMS #6 MRM of 4 Channels ES- 9.91 498 > 78 10o0] i I ..... T' ,', _' , , ,, "[ .... 2.00 j .... 4.00 't .... ] .... 8.00 26767_ I .... j r, r', [" , I ' ' I .... 8.00 10.00 1.33e5Area '[ .... _Time 12,00 1111_ Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Page 71 _# Study No.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslyr_x\Fluorochemlcals. PRO\SampleDB\073103AR Decatur BC Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6kMasslymxkFluorochemicals.PROkMsthDBkDecatur BC 080103 Sun Aug 03 07:11:59 2003 Printed: Wed Au_ 06 11:04:02 2003 Name: 073103AR-136 Text : I: C8 Acid (PFOA) XC072503-6, 1000 ng/L Standard 073103AR-136 Sm (Mn, 2x3) 4 477931 04-Aug-2003 07:52:21 LC/MS/MS #6] MRM of 4 Channels ES- 2.78e6 Area l,oo 1 413> 6! ! 0 i , ,., , ,_-_, , , _ .... _ .... I .... I .... _ .... _ .... _ .... I .... , .... r .... t Time 2.00 4.00 6.00 8.00 10.00 12.00 _ 2:C6 Sulfonate (PFHS) XC072503-6, 1000 ng/h Standard 073103AR-136 Sm (Mn, 2x3) 04-Aug-2003 07:52:21 LC/MS/MS #6 MRM of 4 Channels ES- 8.96 399 > 80 10o]0 0 .... .... , .... 7 .... J .... , .... J .... ,'''' 808181 _ ' ' ' _' ",' r .... 4,81e5Area i "' .'_Time 2.00 4.00 6.00 8.00 10.00 12.00 3:C8 Sulfonate (PFOS', XC072503-6, 1000 n_L Standard 073103AR-136 Sm (Mn, 2x3) 5315 04-Aug-2003 07:52:21 LC/MS/MS #6 MRM of 4 Channels ES- 3.02e5 %1 0 I ' r t ' , ' ' : ' .... "' 2.00 ' I .... , .... 4.00 } .... , .... 6.00 _ .... [' ' ' I I _ .... 8.00 [ .... 10.00 Area _ .... ,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Q_antify Sample Report %_ Study NO.:L34910, Set No.:073103AR, Ext.Date:07/31/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\073103AR Tue Aug 05 06:59:53 2003 P:\Data\LCMSMS6\Masslyrn_\Fluorochamicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Wed Aug 06 11:04:02 2003 Page 72 Decatur BC BC 080103 Name: 073103AR-136 Text : 4 : PFOSA XC072503-6, 1000 ng/L Standard 073103AR-136 Sm (Mn, 2x3) 04-Aug-2003 07:52:21 LC/MS/MS #6 I MRM of 4 Channels ES- 9.90 498 > 78 1(o/1 190680_ 9.76e5Area i 0 t .... _ .... .... .... ,.... .... _ .... d ' ,, _,,, _ .... i , , r, , .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Sponsor Study No: E,xygen Study No: Anatyr,': Ions Monitored: Site: NA 134910 PFOS 499 -> 99 Decatur Baker's Creek RAW DATA REPORT Limit of Quantitaoon: injectlDn Volume: Man'/x: Sample Volume: Final Volmv_: 50 ppt 15 _L Water 40.0 mL 5.0 mL Set No: Analyst: Instrument Type: Extraction Date; Analyzed on: 080603A Karen Risha LC/MS/MS Unit # 6 07/31103 & 08106/03 08/06/03 Exygea ID XC072503-0 XC072503-I XC072503-2 XC072503-3 Sponsor ID Sample Code CS CS C.S CS Run No. 080603A-1001 080603A-1002 080603A- I003 080603A- 1004 Std. Cone. (ppt) 0 25 50 100 Ehlution Fact_ Peak Area 0 1238 2570 4455 Analyte Found (ppt) Amount Added (ppt) Recovery (%) XC072503-4 CS 080603A-1005 250 10551 XC072503-5 CS 080603A- I006 500 22336 i i XC072503-6 CS 080603A-I 007 1000 43039 0106020 Control C 080003A-1008 0 ND 0106020 Spk A LCS 080603A-I009 2436 51.3 50 103 0106020 Spk B LCS 080603A-1010 21693 490 500 98 L34910-12 L34910-16 Spk E Spk F BC2 5W-06 Ouffall to River SW-25 LF 080603A-1011 LF 080603A-1012 101 22031 49800 25000 95 200 18543 " 50000 V L.34910-16 Spk F Ouffall to River SW-25 LF 080603A-1013 100 35655 80900 50000 99 XC072503-1 CS 080603A-1014 25 1229 XC072503-2 XC072503-3 CS 080603A-1015 50 CS 080603A- |016 10(3 2338 4928 1..34910-1 BC2 S W-.O4 S 080603A-1017 - 100 5243 11500 t.34910-1 gep 1-.34910-12 BC2 SW-04 BC'2 5W-06 S 080603A-1018 S 080603A-1019 I00 5235 100 11612 I 15i30 26100 1-34910-i2 Rep 1.34910-15 X1C3047921500-31-34 BC2 SW-06 BC2 SW-06 Dup BC2 SW-06 Low Spk 5 080603A.1020 100 11897 26700 5; 080603A-1021 100 11205 25100 CFSF 080603A-10212023 250 I0-0 140285073 32100 100 6000 XC0725O3-5 XC071003-6 CS 080603A-1024 CS 080603A- 1025 Analym Found (ppt) = (peak area - intercept) / slope x DF Rect_very (%) = Iamfl)'te found (ppt)-a.uat_te found [u coawa[ (ppt)] 7, t00 amount added (ppt) 500 10(30 23323 44271 _ : I itxear (I/x weighted) Internep_ = 184..3].2 Slope = 43.8624 Cool. Of Dot. -- 0.998804 C5 = Calibration standard LF =Lab fortified sample S = Sample CK = Cheek Start "dard LCS = Laboratory Control Spike ND = Not detected = Response between 0 and 25 ppt NQ = Not quantifiable = Response between 25 ppt and LOQ (50 ppt) *Sample +Sample was anaJyzed with several dilufon factors. TI_ appropnam result is repot_d. residue significantly exceeds _he spiking level; therefore, aa accuraz recovery cannot be calculated. /I Spreadsheet prepared by: II ii i 058RPhonc:h '17 a s _ A _,:C H State College, PA 16801 Fax: 814-231-1580 Exygen Study Number: Sponsor Study/Protocol No: Internal Chain of Custody/Fortification . L34910 NA Sheet Matrix: Water The samples listed below were removed--_romrefrigerator No. _" Time 1_3_ Date t3__blO"_ , 1_)_ Initials /''?x"- "i1 CLIENT SAMPLE ID I EXYGEN ID Nqo_IBER I VOLU_.IE !mL) [ FORTIFICATION (ng) na ' 0106020 Control I 40.0 na 0106020 Spk A 40.0 2.0 na 0106020 Sp.k B 40.0 20.0 BC2 SW-06 L34910-12 Spk E 40.0 Outfali to River SW-25 L34910-16 Spk F 40.0 . 1000,0 2000,0 0106020 Spk AB L34910-12SpkE " Spiking Solution Used FF006611110033--t2((II000 nt_tg/m/mLL)) F060203-I (t0000a_/mL) Volume Used for Spiking 200 _FL (200 [F_LLmicropipe.et)t .I t00bL(200pLmicropipet / .In itial/Date _ _' /0O_[_'1/(__(___ _-' /D_lt_,_.._ 0 I All samples were measured: Time 12t'_O Date _ _IC)'_ After measuring sample,,;were returned to refrigerator No. Initials Time \56 Comments: Date .__.__ Initials _- 200_t. of250rng/mLsc_ium_osu_fateWasa0._edtoans_ap[es_fo_ts" t_k_ing, tnida[s/Datree; :v _ k.) _e]_103 Data Set: _ Data Set: -- Initials/Date: Initials/Date: .,.W / - / .'- l Set extractioNanalysis data verified by: &_ Date: ,July 26. 200116 ~ 22 io]l = BL 2s 2 >) = i : 5d : I]2,14 4 E 414 2: :3 z z Cf MHI, 5% 2 3 [83 SPIT s 18 = pre 11 iz oz dB 7 ii 2 : [ wiid: ESEuEaRlle Zi TL ern LT Cs FHT FRI & OF [1 SEA3:NE2 E1E98E 0 5 FP i3 ii : FL F2E2 1HI d 4 FI =: Fr iiT 1d a - o?ci` Zi i : dl 3 2 i il fal fs iH3E9L7E 8: 288 35 fBiRgE:E 232% 2E __ iiiii iiii ii i I IIIII II ,, 0 _9 {D rl cD CD_ c_ LC/MS/MS SYSTEM AND OPERATING CONDITIONS LI_j,Y Sponsor ProtocoI No: NA Exy_en Study No: L34910 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #6) Computer: Software: COMPAQ Professional Workstation AP200 Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 HPLC Equipment: Hewlett Packard (HP) Series 1100 I-_ Bin Pump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column: Genesis C-8, 5 cm x 2.1 mm i.d. x 4 _ (Exygen ID: 74A) (JONESCHROMATOGRAPHY: Part No. FK5962E) Mobile Phase (A) : 2 mM Ammonium Acetate in Type I Water MAnoabliylset:Phase (B): MKaertehnanRolisha @_ C)_I_I_ J Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 NOTE: The next 3 pages are computer generated printouts from the masslynx software program. The pages contain the instrument settings used for the analysis of this data set. / All Handwritten Peak ID's by: _I0_[/Y "5 O' _ Scanning Method Report Method: Last Modified: C:\NASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\C6 Thu Jul 31 16:23:50 2003 C8 SULF C8 ACID PFOSA Page 1 Printed: Wed Aug 06 13:15:53 2003 _'0_ Solvent Delay ( mins ) : 0.00 Analog Channel Function :1 4 : Unused _ of 4 Mass Pairs ( ESP- ) Inter Channel Delay ( Sess ) : Span ( Oaltons ) : Start Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.CO 0.00 12.00 1 Dwell (Secs) Coll Energy (eV) Cone ( V ) 1 399.00 80.00 0.20 35 50 2 413.00 369.00 0.20 i0 i0 i 3 498.00 78.00 0.20 30 50 4 499.00 99.00 0.20 40 30 _W,r Method Report Method File: Last Modified: C:\MASSLYITA\FLUOROCHEMICALS.PRO\ACQU]3B\pfbs Wednesday, August 06, 2003 13:15:26 water Page 1 ,. Printed: HP!I00 LC Pump Initial Conditions Solvents A% B% C% D% Wednesday, August 06, 2003 13:16:00 90.0 !0.0 0.0 0.0 ____ Flow Stop Min Max Oven Oven (m!/min) Time (mins) Pressure (bar) Pressure (bar) Temperature Left(_C) Temperature Right(C) 0.300 20.0 0 400 35.0 35.0 HPll00 LC Pump Gradient Timetable The gradient Timetable contains 8 entries which are : Time A% B% C% D% Flow Pressure 0.00 90 0 i0 0 00 0.0 0.300 400 2.00 90 0 I0 0 00 0.0 0.300 400 5.00 I0 0 90 0 00 0.0 0.300 400 J 9.00 i0 0 90 0 00 0.0 0.300 400 9.50 00 i00 0 00 0.0 0.300 400 14.00 00 i00 0 00 0.0 0.300 400 14.50 90 0 i0 0 00 0.0 0.300 400 20.00 90 0 i0 0 00 0.0 0.300 400 HPll00 LC Pump External. Event Timetable The Timetable contains 6 entries which are : Time Initial 0.00 0.05 0.I0 11.90 12.00 Column Switch Off Off Off Off[ Off Off[ Contactl Off On Off Off Off Off Contact2 Off Off Off On Off Off Contact3 Off Off Off Off On Off Contact4 Off Off Off Off Off Off HPll00 Autosampler Initial Conditions Draw Speed Eject Speed (_l/min) Draw Position (mm} Stop Time (mins) Injection Volume(_l) Vial Nu_nloer 200.0 200 0.50 20.00 15.0 82 _J I_ Tuning Method Report Method : C :\MASSLYIqX\FLUOROCHEMICALS. PRO\ACQUDB\FLUOROCHEMS Printed: Wed Aug 06 13:!9:13 2003 gU[J__0A_I_'05. Page 1 Dau 395.00 329 33[ SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture i Hexapole 2 Source Block Desolvation Temp. Temp. SeU 3.00 20 0.0 0.0 0.0 i00 300 Rdbk -2.93 -43 99 299 Pressures Analyser Gas Cell Vacuum Rdbk OFF 4.0e-3 AnalYser LM Res 1 HM Res 1 IEnergy ! Entrance Collision Exit LM Res 2 HM Res 2 iEnergy 2 Multiplier Gas Flows Cone Gas Desolvation V Set 14,0 14.0 1.0 -2 15 2 14.0 14.0 2.0 650 Rdbk 24 29 27 -646 Rdbk 132.1 770.3 Quantify Calibration Report _ Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Axlalyst:K.Risha Page 1 Calibration: Last modified: P:\Data\LCMSMS6\Masslynx\Fl_orochemicals.PRO\CurveDB\080603A Thu Aug 07 12:27:57 2003 Decatur BC Printed: Thu Aug 07 12:49:55 2003 ___0_ U name: (PFOS) Coefficient of Determination: 0.998804 Calibration curve: 43.8624" x + 184.312 Response type: External Std, Area ICCuormvepotuynped: ILinear, OCr8iginS:ulEfxocnluadtee, Weighting: l/x, Axis trans: None 4.43e4- x Response- r ,. I//0-_ l I 0.0 200.0 _ / 400.0 l _ 600.0 L I 800.0 Exygen Research, 3058 Research Drive, State College, PA 16801 i _ng/L 1000.0 Quantify Sample Report %_j Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 1 Sample List: Last modified: Method: Last modified: P:kData\LCMSMS6\MasslynxkFluorochemicals.PR0\San_leDB\080603A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6kMasslynxkFluorochemicals.PROiMethDBkPFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Job Code: Printed: Thu Aug 0V 12:49:56 200a _n#_o_A-,_,To;_,.____.____==_ Name: 080603A-1001 Text : i: C8 Sulfonate (PFOS) XC072503-0, 0 ng/L Standard 06-Aug-2003 14:57:47 LC/MS/MS #6I 080603A-11000171.29S(Mmn_, 2x3) /I _/ MRM of 4 Channels4>9E9S99 949 1.71e3, 270:_Z-'/'68' 3"68_:_ 1"43 56_0 "74' ['O2 '.C)0" ' 10100 ' Tlme ' V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 2 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080603A Thu Aug 07 08:12:08 2003 P:kData\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-I002 Text : i: C8 Sulfonate (PFOS) XC072503-1, 25 ng/L Standard 080603A-1002 Sm (Mn,2x3) 06-Aug-2003 15:19:26_ LC/MS/MS #6j MRM of 4 Channels ES- lOOj O 9.35 499 > 99t g0o ............ _' 2.00 4.00 , .... _ .... _. .... , .... ," ' ' ' r .... , .... 6.00 8.00 10.00 Time %.# Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %IJ Study No.:L3_910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 3 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals. PRO\SampleDB\080603A Decatur BC Thu Aug 07 08:12:08 2003 P:kData\LCMSMS6\Masslyn_kFluorochemlcals.PRO\MethDBkPFOS only 080603 Thu Aug 07 08:11:08 2003 Printed: Thu Aug 07 12:49:56 2003 Naune : 080603A-1003 Text : i: C8 Sulfonate (PFOS) XC072503-2, 50 ng/L Standard 080603A-1003 Sm (Mn, 2x3) 00_, 1 9.32 2570-A 06-Aug-2003 15:41:07 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 1.18e4 %l_ .j_ L Area 1 Or, ,-7-;_,i,, _.,,,, ,---1-.... i .... _ , , , , , .... J .... _ .... ,' ''' ,.... ,.... Time 2.00 4.00 6.00 8.00 10.00 qlJ Exygen Research, 3058 Research Drive, State College, PA 16801 Qua/itify Sample Report %_ Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 4 Sample List: Last modified: Method: Last mmdified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080603A Thu Aug 07 08:12:08 2003 P:kDatakLCMSMS6kMasslynxkFluoroch_unicals.PROkMethDBkPFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-I004 Text : : C8 Sulfonate {PFOS) XC072503-3, 100 ng/L Standard 080603A-1004 Sm (Mn, 2x3) 1 06-Aug-2003 16:02:511 LC/MS/MS #6I MRM of 4 Channels ES- 44 1.99e4 Area ! O0o/l ........... _ .... 'L.,,, L .... L .... _ .... t .... 9.3_5._..j_. _ 2.00 4.00 &00 8.00 10.00 499Ti>m9e9} V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080603A, Ext.Date:07/31 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals. Thu Aug 07 08:12:08 2003 P:\DatakLCMSMS6\Massly_x\Fluorochemicals. Thu Aug 07 08:11:08 2003 Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-I005 Text : i: C8 Sulfonate (PFOS) XC072503-4, 250 ng/L Standard 080603A-1005 Sm (Mn, 2x3) 10 & 08/06/03, Analyst:K.Risha PR0\San_leDB\080603A Page 5 Decatur BC PRO\MethDB\PFOS only 080603 1055 t 06-Aug-2003 16:24:39 LC/MS/MS #6' MRM of 4 Channels ES- I 4.71e4/ C .... ,r-_>_',2.(7r0"-,' ' ' , .... 4.00._... I .... 6.00_,,., r _ .... 8.00._... _ .... 10.00'-'-_' '-_=' _--' Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06103, Analyst:K.Risha Page 6 Sample List: Last modified: Method: Last modified: Job Code: P:\DataXLCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080603A Thu Aug 07 08:12:08 2003 P:XData\LCMSMS6\Massly_x\Fluorochemicals.PR0\MethnB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 Nan%e : 080603A-I006 Text : : C8 Sulfonate (PFOS) XC072503-5, 500 ng/L Standard 080603A-1006 Sm (Mn, 2x3) 06-Aug-2003 16:46:1 ! LC/MS/MS #61 MRM of 4 Channels ES- I 9.31 499 > 99I 101Q1 ' 0 t ' ', , ,' "_--_ r , I .... 2.00 , .... I .... 4.00 I .... [ .... 6.00 223361 I .... I = r "1 ; t .... _,''' 8.00 10.00 9.64e4Area , .... Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report I_ Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 7 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080603A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslynx\Fluorochem/cals.PRO\MethDB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-I007 Text : l: C8 Sulfonate (PFOS) XC072503-6, 1000 ng/L Standard 080603A-1007 Sm (Mn, 2x3) 100_ % 9.33 4303 06-Aug-2003 17:08:00_ LC/MS/MS #6! MRM of 4 Channels ES499 > 99 1.83e5 i 01 .... i _, , , i .... 2.00 i .... _ .... 4.00 _, , , , _ .... 6.00 L,, ,_ .... _ .... L ,', , , _ .... 8.00 10.00 Time %1# Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %_ Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/05/03, Analyst:K.Risha Page 8 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080603A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 Nan%e : 080603A-I008 Text : i: C8 Sulfonate (2FOS) 0106020 Control 080603A-1008 Sm (Mn, 2x3) 10" 1.,30 06-Aug-2003 17:29:43 LC/MS/MS #6 MRM of 4 Channels ES- I' 499 > 99 fv_ o _/--_ _ / \\ 3.37 4 38 4 97 ....... 4" 9.41 10A47/10.72 1/1.69 i (} .... _',', , .... , .... _ .... i .... , ' ' ' , .... J' "'-"l .... , .... , .... 2.00 4.00 6.00 8.00 10.00 Time V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %_ Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 9 Sample List: Last modified: Method: Last modified: Job Code: _:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080603A Thu Aug 07 08:12:08 2003 P:\DatakLCMSMS6kMasslyr_\Fluorocheraicals.PRO\MethDB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-I009 Text : i: C8 Sulfonate (PFOS) 0106020 Spk A, 50 ng/L 080603A-1009 Sm (Mn, 2x3) 06-Aug-20L0C3/MS1/7M:5S1:2#_6 I MRM of 4 Channels ES- I 9.30 499 > 991 1.06e4 1to/i_ - .21 2.00 4.00 6.00 8.00 10.00 Area ii Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report t_ Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06103, Analyst:K.Risha Page i0 Sample List: Last modified: Method: Last modified: Job Code: P:kData\LCMSMS6\M_sslyr=x\Fluorochemicals.PROkSam_leDB\0B0603A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslyrux\Fluorochemicals.PRO\MethDB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-I010 Text : i: C8 Sulfonate (PFOS) 0106020 Spk B, 500 ng/L 080603A-1010 Sm (Mn, 2x3) 0S-Aug-2003 18:13:04_ LC/MS/MS #6 I MRM of 4 Channels ES- I 9.31 499 > 99 % 100_1 216931 9.5A8rea4 !! 0_ .... ,_,, _-, ,,. _ .... , , ,-, , , .... _ .... _, '.-,, _,, ",, j,, ,-,_, .... _ .... Time 2.00 4.00 6.00 8.00 10.00 %=J Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page Ii Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslyr_\Fluorochemlcals.PR0\Sa/npleDB\080603A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslyru_\Fluorochemicals. PRO\MethDB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-I011 Text : i: C8 Sulfonate (PFOS) L34910-12 Spk E, 25000 rig/L, DF=100 080603A-1011 Sm (Mn, 2x3) 06-Aug-2003 18:34:45 LC/MS/MS #6 MRM of 4 Channels ES- 9.33 499 > 9 Area i 100_ 22031_ 9.3684 %0 j .... _ , , , , , , , i .... , .... , .... , _'' , .... _ .... , .... I .... _ .... Time i 2.00 4.00 6.00 8.00 10.00 %,,a' Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report ,,_ Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 12 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080603A Thu Aug 07 08:12:08 2003 P:\DatakLCMSMS6\MasslynxkFluorochemicals.PRO\Metb-DBkPFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-I012 Text : : C8 Sulfonate (PFOS) L34910-16 Spk F, 50000 ng/L, DF=200 080603A-1012 Sm (Mn, 2x3) 0S-Aug-2003 18:56:25 LC/MS/MS #6 MRM of 4 Channels ES- 9.32 499 > 99 1001%1 0" .... J .... I .... 2.00 4 .... I .... 4.00 _ .... J .... 6.00 1854a_ i .... _ .... i .... l .... 8.00 10.00 7.99e4Area '1 ' ' ' Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report *_r Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 13 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080603A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\MethDB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-1013 Text : i: C8 Sulfona_e (PFOS) L34910-16 Spk F, 50000 rig/L, DF=100 080603A-1013 Sm (Mn, 2x3) 06-Aug-2003 19:18:10_ LC/MS/MS #6 I MRM of 4 Channels ES- I 9.29 499 > 99/ q 1(_"/'l 35655j_ Area i It 1.54e5 0 _ .... .... r .... , .... J .... _ .... , .... , .... , .... , .... , .... , .... 2.00 4.00 6.00 8.00 10.00 Time ' I l,w, %,,,# Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify sample Report _ Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 14 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Mass!ynx\Fluorochemicals.PRO\SampleDB\080603A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PR0\MethDB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 Name: Text: 080603A-I014 i: C8 Sulfonate (PFOS) X0072503-1, 25 ng/k Standard 080603A-1014 Sm (Mn, 2x3) 100-_ 1 9.36 1229] 06-Aug-2003 19:39:56 LC/MS/MS #6 MRM of 4 Channels ES- 499 > 99 5.58e3 % 'i !_ 0 _.... J ' ' _ ,.... 2.00 i .... _ .... 4.00 _ i .... _ .... 6.00 , .... , .... 8.00 i .... _" ' ....... 10.00 Area Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample ReDort _ Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 15 Sar_ple List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorocheunicals.PRO\Sam_leDB\080603A Thu Aug 07 08:12:08 2003 P:XDataXLCMSMS6kMasslynx\Fluorochemicals.PRO\MethDBkPFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-I015 Text : i: C8 Sulfonate (PFOS) XC072503-2, 50 ng/L Standard 080603A-1015 Sm (Mn, 2x3) ] % 06-Aug-2003 20:01:40 LC/MS/MS #6 MRM of 4 Channels ES- 9.36 499 > 99 Area i _ 100_ Or-_-_. _' ,_,_____,_. 2.00 231_ 1.08e4 , _ .... _ .... , .... , .... _,,-, ,-_ .... _ .... L.... Time 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _m_ Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 16 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080603A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDBkPFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-I016 Text : I: C8 Sulfonate (PFOS) XC072503-3, 100 ng/L Standard 080603A-1016 Sm (Mn, 2x3) l n_ 06-Aug-2003 20:23:22 LC/MS/MS #6 MRM of 4 Channels ES- 9.35 499 > 99 Area ! ....... , .... ,.... _ .... ,.... , .... , .... c .... 4__d._... _.... r_, =2T.2im0ee4 2.00 4.00 6.00 8.00 10.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 17 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080603A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslyr_\Fluorochemicals.PRO\MethDB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 Narae : 080603A-I017 Text : i: C8 Sulfonate (PFOS) L34910-1, DF=100 080603A-1017 Sm (Mn, 2x3) 06-Aug-2003 20:45:02_ LC/MS/MS #6 MRM of 4 ChannelsES- 9.33 499 > 99 Area i J I 1_1 '-_'7--T--T--I .... 2.00 I .... I .... 4.00 I .... I .... 6.00 524_ 2.2184 I .... I .... 1 .... , ' ,--;-_7_,--"_"-_,,Time 8.00 10.00 _J Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 18 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080603A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslym.x\Fluorochemicals.PRO\MethDB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 Na/ne : 080603A-I018 Text : i: C8 Sulfonate (PFOS) L34910-1 Rep, DF=100 080603A-1018 Sm (Mn, 2x3) 06-Aug-2003 21:06:44{ LC/MS/MS #6I MRM of 4 Channels ES- I 9.35 499 > 991 i 10/00__Ji._. _-_ ,,, -_q---_-_-. i .... _.... 2.00 4.00 : .... , .... ; .... , .... 523J5L.... _ .... , .... 2T.4Aim1reea4 6.00 8,00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _._ Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 19 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080603A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\MethDB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-I019 Text : i: C8 Sulfonate (PFOS) L34910-12, DF=100 080603A-1019 Sm (Mn, 2x3) 100_. 4 %_ ] _i .... J"' ' ' ' , .... 2.00 ,' "L ' J .... 4.00 _-' ' ' ' _ .... 6.00 9.31 11612] 06-Aug-2003 21:28:28_ LC/MS/MS #6i MRM of 4 Channels ES-I 4959.0>49e94I! J .... ,.... 8.00 L L.... _ ' ' ' _ * ' ' 10.00 Areai Time V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 20 San_le List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080603A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslynx\Fluorochea%icals.PROkMethDBkPFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-I020 Text : I: C8 Sulfonate (PFOS) L34910-12 Rep, DF=100 080603A-1020 Sm (Mn, 2x3) 10J0-_ 06-Aug-2003 21:50:16 LC/MS/MS #6 . MRM of 4 Channels ES- I 19.321II877] 4995>.2999ei 4 %1 j_ 2.00 4.00 6.00 8.00 10.00 Area _ J Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 21 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\Sam_leDB\080603A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals. PRO\MethDBkPFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-I021 Text : i: C8 Sulfonate (PFOS) L34910-15, DF=100 080603A-1021 Sm (Mn, 2x3) 06-Aug-2003 22:12:03_ LC/MS/MS #6J MRM of 4 Channels ES- 9.33 499 > 9 0 t .... .... r .... 2.00 _ .... _ .... 4.00 , .... 'J .... 6.00 _ .... ,'_ ............. 8.00 10.00 _-' Time V I Exygen Research, 3058 Research Drive, State College, PA 16801 _,_r Quaultify Sample Study No.:L34910, Report Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080603A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\MasslyrLx\Fluorochemicals.PRO\MethDB\PFOS Thu Aug 07 08:11:08 2003 only Page 22 Decatur BC 080603 Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-I022 Text : : C8 Sulfonate (PFOS) L34910-13, DF=100 080603A-1022 Sm (Mn, 2x3) 06-Aug-2003 22:33:46_ LC/MS/MS #6I MRM of 4 Channels ES- I 9.36 499 > 99I 1C10y L.... _ .... 2.00 _ .... , .... 4.00 , .... _. ..j 6.00 .... .... 1425_7..j._.L , .... 8.00 10.00 _ .... 6T.1im3ee4Area Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %_ Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 23 Sample List: Last modified: Method: Last modified: Job Cede: P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\Sam_leDB\080603A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslyzuc\Fluorochemlcals.PRO\MethDB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 Name: 080603A-I023 Text : i: C8 Sulfonate (PFOS) XC072503-4, 250 ng/L Standard 080603A-1023 Sm (Mn,2x3) 06-Aug-2003 22:55:27 LC/MS/MS #6 MRM of 4 Channels ES- 9.34 499 > 99 Area i 0% , ,, ,_-/_'>,, , ,.., , , _ .... r, ,_, _ .... , .... 2.00 4.00 6.00 i .... _ .... 8.00 i .... = , , ,"_T .... 10.00 Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quaultify Sau_le Report %q_ Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 24 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\San_leDB\O80603A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\MethDB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 Name: Text: 080603A-I024 i: C8 Sulfona_e (PFOS) XC072503-5, , t 500 ng/L Standard 100_ 9.33 23323 06-Aug-2003 23:17:07 LC/MS/MS #6 499 > 991 9.98e4 % l Area : 0L, , ,T j,_c>-,. , . ,--, i .... , ,, ,-, i .... _ .... i .... "_ .... i .... ,_,, ,l .... Time 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report 51W Study No.:L34910, Set No.:080603A, Ext.Date:07/31 & 08/06/03, Analyst:K.Risha Page 25 Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6kMasslynx\Fluorochemicals.PRO\SampleDB\080603A Thu Aug 07 08:12:08 2003 P:\Data\LCMSMS6kMasslynx\Fluorochemicals.PRO\MethDB\PFOS Thu Aug 07 08:11:08 2003 Decatur BC only 080603 Printed: Thu Aug 07 12:49:56 2003 Name: Text: 080603A-I025 i: C8 Su!fonate (PFOS) XC072503-6, 1000 ng/L Standard 080603A-1025 Sm (Mn, 2x3) 06-Aug-2003 23:38:5_ LC/MS/MS #6 MRM of 4 Channels ES- 44271 1.91e5 Area z t 100_ 9,31 499>99 O" .... _,_, _ , _ .... i .... i,,,-, _ .... i .... _,, _,,,_ .... _ .... _ .... _ .... 2.00 4.00 6.00 8.00 10.00 Time Exygen Research, 3058 Research Drive, State College, PA 16801 SECTION E II II I I Sponsor Srady No; Exygcn Study No: A.nalyte: ions Motxitored: Site: NA I.,34910 PFOA 413 -> 369 Decatur Baket's Creei IL_,W DATA REPORT Limit of Qulmfitation: Injection Volume: Matrix: Sample Weight: Fioa/Volume: 50 irpt 15 pL Soil 5.0 g 3.0 mL Set No: Analyse Lastn_ment Type: Extr_tion Analyzed Dam; on: 080103A Karen Risha LCMSMS 06 08/'01/113 08,,02,'03 Exygen Sponsor Sample Run Std. Cone. Diiufion Peak Analyt* Found Amount Added Recovery A.nalym Fotmd Total Solids Amdym Foxtul (ppb) ID XC072503-0 XC072503-1 XC1172503-2 XC072503-3 XC072503M ID Code No. (ppt) Factor Area (ppt) (ppt) ... (%) . fppb) ,. (%} DrT.Wci_ht CS 080103A-2001 0 333 CS 080103,'k-2002 7.5 9882 C,S 080103A-2003 50 |7917 CS 080103A-2004 100 34827 C3 080103A-2005 250 78794 XC072503-5 XC072503-6 CS 080103A-2006 500 CS 0g0103 A.2007 1000 I71634 315768 Methaaol Wash C 080103A-2008 525 ! Reagent Blank na C 080103A-2009 318 ND ] Reagent Spk A aa LCS 08Ot03A-2010 18939 55.3 50 III Reagent Spk B XC072503-1 na LC.S 080103A.2011 163063 536 500 107 CS 080103A-2012 23 9820 1-34910-5 Spk C L34910.10 Spk D L34910-11 SpkE BC'2 SED-04 BC2 SED-05 BC2 SED-06 LF 080103A.2013 LF 080103A-2014 I.,F 0_.0103A-20 l 5 10 157971 5190 5000 96 10 166134 5460 5000 96 i0 187666 6150 50_3 88" L34910-20 Spk F Outfall to Rivet SED-25 _f XC072503-2 LF 080103A.2016 10 179090 5890 5000 91 ^ CS 080103A-2017 50 18190 L34910,5 BC'2 SF,D-O4 S 080103A-2018 1 1154.51 377 3.02 69,96 4.31 1.34910-5 Pep 1...34910-10 BC2 SED-04 BC'2 SED-05 S 080103A-2019 S 080103A-2020 l 82762 268 1 193055 642 2.14 69.96 5.14. 69.5.* 3.0t5 7.39 L34910-10 Rep XC072503-3 XCAY/2503 -4 L34910.11 BC2 SED4_5 BC"2 SED436 S 080103A-2021 1 167826 551 CS 080103A-2022 I00 33_0 CS 080103A-2023 250 79282 S 080103A.2024 1 473416 * 4.41 69.54 6.34 60.41 L34910-11 Rep L34910-20 BC2 SF,.IN06 Outf'all toRiverSED-25 S 080103A-2025 S 0_ 103A-7.026 l 463017 1 404209 60.41 63.27 1..34910.-20 Pep Outfall to Kiver SED-2,5 S 080103A-2027 1 301201 " L.3_.910-21 XC072503-5 Outfall to River SED-25 Dup S 080103A-1:02_ 1 532619 " CS 050103A-2029 500 140009 XC072303-6 CS 080103A-2030 1000 273386 63.27 6"].43 Analyte Found (ppt) = (peak area - mtercep0 / slope x DF Ri_=ov_ (%) = (;malym fotmd (ppt)-anaJyte found in control (pp_)] x 100 amotmt added (ppt) Standard Cutwe : L_ear (l/x weighmd) Lmen:ept = 2.344.75 Slope = 300.076 CccL 'Of D,_. = 0.988097 Analyt_ Found (ppb) - [analyte found (PPO x volume extracted (0.04L.)]I sample *eight (5 g) Analyte Found (pgb) dr'/weight = analyte fotmd (p_b) x (l(]0% I total aolida (%)) CS = Calibration standard C = Control sample S = Sample LF = Lab fortif;ed sample FF = Field fortified sample LCS = Laboratory Control Spi_ CK = C:a_k Standard ND = Not detected = R_spo_.c between 0 and _ ppt NQ = Not quantifiable = Response between 25 ppt and LOQ (50 ppt) Sample requires dilutiom See data set 080103AR. _1t_ "Sample wa_ corrected using the data found in set O80103AR. Spreadsheet prepared by: _/_ {)_'_ Sponsor Study No: Exygen Study No: AnaJyte: lore Monitored: Site: NA L34910 PI,'I:IS 399 -> 80 Decarta- Baker's Creek RAW DATA REPORT limit of Quanfitafion: Ink:orion V01umc: Matrix: Sample Weight: P/aal Volume: 50 ppt 15 _A. Sod 5.0 g 5.0 m/. Set No: Analyst: Lnstruamnt Type: Extraclioo Date: Ana/yzed on: 080103A Kaxcn Risha LCMSMS #6 08/01/03 08/02/03 Exygen ID XC072503-O XCOT'2503- I XCOT2503-2 XC072503-3 XC072303-4 XC072503-5 Sponsor ID Sample Code CS CS CS CS CS CS Run No. 080103A-2001 080103A-2002 080103A-2003 080103A-2004 080103A-2005 080103A-2006 Std. Cone, (ppt) 0 25 50 100 250 500 Dilulaoa Factor Peak Area 0 1572 3699 6481 15770 31281 A.nzlyte Found (ppt) Amount Added (ppt) Recovery (%) Analyte Found (ppb) Total Solids (%) A._alyte Found (ppb) Dry Wei[ht XC072503-6 Methanol Wash Reagent Blank Reagent 5pk A Reagent Spk B XC072503-1 L34910-5 Spk C L349lO-10 Spk D na na na BC2 SED-04 BC2 SED-O5 C_.5 080103A-2007 I000 C 080103A-2008 C 080103A-2009 LCS 080103A-2010 LCS 080103A-2011 CS 080103A-2012 25 58308 0 0 ND 3457 52.0 50 104 31000 533 500 107 1765 LF 080103A-2013 LF 080103A-2014 10 30746 5280 5000 104 10 32192 5330 5000 107 _ L.34910-] l SpkE BC2 SED-06 L34910-20 $pk F Outfali m Rivet SED-25 XC072503-2 L34910-5 BC'2 SED-04 LF 080103A-2015 LF 080103A-2016 CS 080103A-2017 S 080103A-2018 10 32334 5560 5000 10 32343 5560 5000 50 3449 1 4534 70.8 105 103 0.57 L34910-5 Rep BC2 SED-04 $ 080103A-2019 1 3439 51.7 0.41 1.34910-10 BC2 SED-05 S 080103A-2020 1 10896 182 1.45 L34910-10 Rgp BC"2 SED-05 S 080103A.20'21 1 12999 218 1.75 XC072503-3 CS 080103A-2022 100 6560 XC072503_ C,S 080103A-2023 250 14801 L34910o I I BC2 SED-06 S 080103A-2024 I 18133 308 2.46 1-34910-11 Pep BC2 SED-.06 S 080103A-2025 1 19203 327 2.61 1.34910420 O.utfidl to Raver SED-25 S 080103A-2026 I 23354 399 3.19 L349i0--20 l_p Outfa_ to P,b,,_etSED*'L5 S 080103A-2027 1 16649 282 2.26 L34910-21 OuffaLI to River SF-,D-25 Dup 8 080103A-2028 I 36172 623 4.98 XC072503-5 CS 080103A-2029 500 28497 XC072503-6 CS 080103A-2030 I000 54198 Analyte Found (ppt) = (peak area- int.e.rt:ept) I slope x DF Recover'/(%) = [analyte found (ppt)-analyte found m control (ppt)J x 100 arnotmt added (ppt} _lada/gl..._a_ hater_pt Slope Cotf. Ofl_L : Linear (fix = 476.906 = 57.3138 = 0.905587 weighted) 69.96 69.96 69.54 69.54 60.41 60.41 63.27 63.27 67.43 0+809 0.591 2.09 2.51 4.08 4.33 5.05 3..57 739 1 , Analyte Found (ppb) = [analyt_ found (ppt) x volu.a_ extra:ted (0.04 L)] / sample weight (5 g) Analyte Fomui (ppb) dry weight = anaiym f_uad (ppb) x (100% I total solids (%)) C.S = CaJibratJiOa :_ta_lard C = Control sample S = Sample LF = Lab fortified sampk: FF = Field fortified sample LCS = Laboratory Control Spik_ CK = Ch_k Smndasd ND Not det_te.d = Respo4as betwet:n 0 and 25 ppt NQ = Not quamifiable = Rcspons_ between 25 ppt amt LOQ (50 ppt) sponsor stray No: Exygeo Study No: Analyte: lons Momtored: Site: NA _910 PFOS 499 -> 99 Decatur Bakers Creek RAW DATA REPORT Lhnit of Quaatitatioa: lnjcefioo Volume: Matrix: Sam.pie Weight: Final Volume: 50 ppt 15 _L Soil 5,0 8 5.0 mL Set No: Analyst: [nsWanaeut Type: F..xu_ti_n Date: Analyzed on: 080103A Karen Rishn LCMSMS #6 08_i/1)3 08/97,._3 Exygen ID XCf172503-0 XC072503-I XC072.503 -2 XC072503.3 XC0"Y2503-4 XC072503-5 Sponsor 1D -. .... _::_ " : ,. .. - Sa_aple Code C.S CS CS CS C,S C,S Rtm No. 080103A-2001 080103A-2002 080103A-2003 080103A-20/M. 0g0103A-2005 080103A-2006 Std. Cone. (ppt) 0 25 . 50 1130 250 500 Diludon Factor Peak Area 0 1018 2077. 3701 9370 19171 Analyte Found (ppt) .- A_ount Added (ppt) l_covery (%) Analyte Found (pph) TotaJ Solids f%) Analyte Fout,d (ppb) Dr_ Weight XC072503-6 CS 080103A.2007 1000 37079 ;. Metha.uot Wasta C 080103A-2008 0 Reagent Blank na C 080103A-2009 0 Nq3 i Reagent Spk A na LC_ 080103A-2010 2011 51.4 50 103 Reagent Spk B XC072.503 -1 na LCS 080103A-2011 17583 496 500 99 CS 080103A-2012 2`5 938 L34910-5 Spk C I..34910-10 Spk D L34910-11 Spk E BC'2 SED-04 BC2 SED-05 BC2 SED-06 LF 080103A-2013 LF 080103A-7.014 LF 080103A-2015 10 22878 6470 `5000 93 ^ 10 26935 7620 5000 95^ 10 336383 * 5000 _ L34910,.20 Spk F Ouffal/to River SED-2.5 LF 080103A-2016 10 72248 5000 XCO72503-2 CS 080103A-2017 50 2233 L.34910-5 BC'2 SED-04 S 080103A-201 g 1 60613 1..34910--5 Rep I..34910-10 BC2 SED-O,4 BC2 SED-05 S 080103A-2019 S 080103A-2020 I 51074 " 1 9384,t * L34910-10 Rep XC072503.8 XC'072503 -4 BC2 SED-05 S 080103A-2021 I 1063,50 CS 080103A-2022 100 3634 CS 080103A-2023 250 8965 I..34910-I 1 BC"2 SED-06 S 080103A-2024 I 2354673 /...3,4910-/1 Rep L349_.0-20 L349 IO-20 Rep BC2 SED.06 Ol.ttfaU to River SEEb2.5 Ouffall to River SED-2.5 S 080103A-202.5 S 080103A-2026 S 08l) i03A-2027 I 17943`53 * 1 418516 * t 287933 * L34910-21 XC072503-5 Ouffall to River SED-2,5 Dup S 080103A-202.$ 1 40987.I * CS 080103A-2029 5(30 17108 XC072,503-6 CS 080103A-2030 1000 32192 69,96 69.96 69.54 69.54 60.41 60.41 63.27 63,27 67.43 Analyte Found (ppt) :_(peak area. intercept) I slope x DF Rr.covery (%) = |a.aalyte ft,,and _ppt)-anal)'te found in control (ppf)] x (_) autlouat added (ppt) _ : Lme,.,_ (l/x weighted) Im_recpt Slope Coef. OlDer. = 208.543 = 35.0593 = 0.9_916 Ana]ym Fo.und (ppb) = [analym found (ppt) x volume extr-_tcd (0.04 L)] / sample weight (.5 8) Anaiyte Found (ppb) d.ry weight _ analyt_ found (ppb) x (100% / total solids (%)) CS _ Ca/ibratioa staz_ard C = Control sample S _ Sample L.F z Lab fortified sample FF J Field foa'tffied _ample LC.S = Laboratory Control Spike CK = C'h_k Standard ND = Not detected z Response _n 0 and 25 ppt NQ _ Not quantifiable z ResDonsc betwe.ea 25 ppt and LOQ (50 ppt) Sample requires dilution. See data set 080103AR. 0 ^Sample was corrected using the data found _n set 080103AR. i i Sponsor Study No: Exygen Study N,J: Anal_e: ]ons Monitored: Site: NA L34910 FOSA 498 -> 78 Decatur Baker's Creek RAW DATA REPORT Limit of Quantflafion: Injection Voltune: Matrx: Saanple Weight: F(nat Volume: 50 ppt 15 }_L Soll 5.0 g 5.0 mr. Set No: Analyst: Instrument Extraction Type: Date: A_alyzed o_: 080l 03A Karen Risha LCMSMS #6 08/01/03 08/02/03 Eaygen Sponsor Std. Analyt_ Amount Analyte Total Analyte Sample Run Cone. Dilution Peak Found Added Recovery Found Solids Found (ppb) ID XC072503-0 XC072503q XC072503-2 XC072503-3 XC072503_4 XC072503-5 XC072503_a Methanol Wash ID Code No. (.ppt) Factor Area (ppt) (ppt t (%) eppb) (%) _ Weight CS 080103A-2001 0 0 CS 08,0 I03 A-2_302 25 3995 CS 080 i 03A-2003 50 CS 080103A-2004 100 7728 15082 CS 080103A-2005 250 CS 080103A-2006 500 36693 72894 CS 080103A-2007 1000 C 080 I03A-2008 137821 0 Reagem alav.k aa C 080 [03A-2009 0 NO ] Reagent Spk A Reagent Spk B XC072503-I na LCS 080103A-2010 6750 43.6 50 87 na LCS 0gO103A-2011 65424 477 500 95 CS 080103A-2012 25 3817 L34910-5 Spk C L34910-10 Spk D L34910-t 1 Spk E L34910-20 Spk F BC2 SED-04 BC2 SED-05 BC2 SED-06 Ouffall lo River SED-25 LF 080103A-2013 LF 080103A-2014 LF 080103A-2015 LF Bg'3103A-2016 I0 79517 5810 5000 98 10 82212 6010 5000 101 10 155090 * 5000 - _.0 _.00640 7370 5000 77 ^ _,,_ XC072503-2 L34910-5 BC2 SED-O4 CS 080103A-2017 50 7957 S 080103A-2018 1 l 218.82 894 7. l 5 69.96 10.2 L34910-5 Rep L34910-10 BC2 SED-04 BC2 SED-05 S 080_03A-2019 S 0g0103A-2020 1 133583 981 I 133763 982 7.84 69.96 7.86 69.54 I 1.2 I 1.3 L34910-I0 Rep XC072503-3 XCO72503-4 L349 IO-I 1 L34910-I l Rep L34910--20 BC2 SED-O5 BC2 SED-O6 BC2 SED-06 Ouffall to River SED-25 S 080103A-2021 I 191201 * CS 080103A-2022 100 14698 CS O80i03A-2023 250 34282 S 080103A-2024 I 1215533 * S 080103A-2025 S 080 I03 A-2026 1 929771 * I 412369 * 69.54 60.4 [ 60.41 63.27 L34910-20 Rep Ouffal[ to River SED-25 S 080103A-2027 1 346884 * L34910-21 Ouffall to River SED-25 Dup S 080103A-2028 1 357273 " XCO72503-5 CS O8Ot 03A-2029 500 67231 XC072503-6 CS 080 t03A-2030 1000 I29_ 18 63.27 - 67.43 Anal_e Found (ppt) = (peak area - intercept) / slope x DF Recovery (%) = fanalvle found (ppt'_-_al',,,te found in cunlxol (ppt)] x 100 amount added (ppt) Standard _ Intercept Slope Coef. OlDer. : Linear (I/x = 849.062 = 135.358 ; 0.996863 weighled) Analyte Found (ppb) = [analyte found (ppt) x volume extracted (O.OZ L)] / sample weight (5 g) Analyte Found (ppb) dry. weight = anaiyte found (ppb) x (1OO% / 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) Sample ^Sample requires dilution. See data sel 080103AR. was corrected using the data found in set 080103AR. Spteadsb.eet p, epaled by:_'_Q 03 & GiEEiEiiiissssh, SiBiEsiRiEsiAssNatagnisd f FSiE3SP3R3EeEIRaEaRaRsFaRiIiRyESd = Haina sd ggBERRfgEegiiiasl FF Rgiidddiddadidids F 8sI] CRA < 4383353838855 jaigrasatasasaidd jeTssTssHesIsssTiiTznEyl siEgiiEiaEiis aw ig i - 3i : g& & _o _Z Z _ o N_ <= Z < _ g O000 ooooo_ 888_88_8_ _,_,_,_,_ ...... _ ................ + -_ E _ E o 'I g E E -en ir....,,... __ RE 5 EA R C H 30 sR se State College, PA 16801 Fax: Internal Chain of Custody/Fortification Sheet Exygea Study Number: L34910 Matrix: Sol____! SpoQsor Study/Protoco| No: NA The samples Listed below were re--movedfrom refrigerator No. 8c21h74D21v03 814-231-1580 Time /3_ __ Date t3_//O,/0_ Initials CLIENT SAMPLE ID EXYGEN ID NUMBER WEIGHT (g) FORTIFICATION .(rig) na Reagent Blank na Reagent Spk A 2.0 na Reagent Spk B 20.0 BC2 SED-04 L34910-5 Spk C 5.0 200.0 BC2 SED-05 L34910-10 Spk D 5.0 _. 200.0 ..... BC2 SED-06 L34910-11 Spk E 5.0 200.0 _. Ouffatl to River SED-25 L34910-20 Spk F 5.0 BC2 SED-0d- L34910-5 5.0 200.0 BC2 SED-O4 L34910-5 Rep . 5.0 !1 BC2 SED-05 L34910-10 5.0 ' _ BC2 SED-05 BC2 SED-06 L34910-10 Rep 5.0 L34910-11 5.0 _ BC2 SED-06 L34910-11 Re.p 5.0 _ Ouffall to River SED-25 L34910-20 ,. 5.0 Ouffall to River SED-25 L34910-20 Rep 5.0 Ouffall to River SED-25 Dup L34910-21 5.0 Reagent Spk A Reagem Spk B L34910-5 Spk C L3d.910-10Spk D L3a910-11 Spk E L349t0-20 Spk F Spiking Solution Used F061103-2 (10 n_mL) F061103-1 (100 n_mL) F060203-2 (11300ng/mL) F060203-2 (1000 a_/mL) F060203-2 (1000 n_/mL) F060203-2 (1000 a_/mL) Volume Used for Spiking 200 pL (200 __. micropipet) 200 IlL (200 pL micropipet). 200 _L (200 _L micropipet) 200 _L (200 _L micro.ipet) 200 pL (200 _L micropipet) 200 I.tL(200 FLLmicrop!pet) Initial/Date _}_2 / 0_101_ ! /0_!0l, _. /I)_3]01 t" /0'0tl)1[ _'_ /O_IOlJC 5 _ /0_ I01/_ All samples were weighed on balance No. 2_ Time /_z4_ Date _/t_/O_/_-- Initials /_ After weighing samples were returned to re/frijgerator No _ Time /.:_ Date (21_]0[/0__ i/ Initials 111 Comments: 200gL of 250mg/mLsodiumthiosulfatewasaddedtoall samplesbeforespiking.Initials/Date_:_ AnalysisSuInmary DataSet _0_/)_ Initials/Date: _ Data Set /)_Jlb_5_ Data Set -- Initials/Date _ Initials/Date x /1611 _ /O_J_t_J_ / Set extraction/analysis data verified by: _]_.f Date; _'/J_iLu"l_y26, 2001/1 -_ nnn HTH + 2% -- 3 |S h 932; 3 Ballin|i | I =ded: s ELIE |P:I EITIROdIeIEdLLOT T[TALTdGFEyedE Sy 5EE g TT: 4 & oji":BEC EH OLE : 113 8% J BIT ER Td: | 5 Epgis E CE CE o 1TEE p HTH H , |PH S z EHH i a0 D 3; | [19R8R45 0 HEE a ag eT 0k|] Jaden |||| (Sil i vo EB i 983 |||] fieelseames 1 12k a ioe "3 B ee 2228cen re g | & coscsscascscsessscssssssacccss | Foon Eo dwn ssl] : 1 2 iinssnrnnanianenyansane inane g2) 33 B | 8 ossenal 288880a 88,088 | ; 5 385533555053088038848 pH 3| rl lbh: mm 5 POH had BOB |g88 ) f5asfiaeosnanayageatdeliligaislansaeisme; |gs80o#5048p2o a0 - PoEmaa | iz sesuuannIdaanaaaacaREReace eos = SI IEBl fon, | & z3 s2gecsoraoreagy 5 ph) EE 3% - | :il5| 3 88 2i 533333333333333533338383885848 I SYPI9EES-ngvnengoo2rIeNaToSSy PEERENAD T HEn TNMTNorealINRIRERR2RINRNNERERR A .o 0 O_ O_ O_ o_ V J d E m o > oog55555555ggggg55555== _ Eeee_eN_Neeeeeeeeeeeeeeeeeeee E _ 000000000000000000000000000000 _ 000 O0 oo 0000000 000000000000 _m LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exygen Study No: L34910 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #6) Computer: COMPAQ Professional Workstation AP200 Software: Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 t-IPLCEquipment: Hewlett Packard (HP) Series 1100 HI' Bin Pump liP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column: Genesis C-8, 5 cm x 2.1 mm i.d. x 4 la (Exygen ID: 74A) (JONESCHROMATOGRAPHY: Part No. FK596ZE) Mobile Phase (AB) :: 2MmetMhanAoml monium Acetate in Type I Water Q_)_b\\ _'2) ] Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 _ Phone: (814) 272-1039 FAX: (814) 231-1580 NOTE: The next 3 pages are computer generated printouts from the masslynx software program. The pages contain the instrument settings used for the analysis of this data set. All HandwrittenPeakID'sby: ,_1_ _-2 Scanning Method Method: Last Modified: Report C:\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\C6 Thu Jul 31 16:23:50 2003 C8 SULF C8 ACID PFOSA Page 1 Printed: Fri Aug 01 15:29:10 2003 _,. Solvent Delay ( mins ) : 0.00 Analog Channel Function :1 4 : Unused MRM of 4 Mass Pairs ( ESP- ) _1_ 5 Inter Channel Span ( Daltons Delay ): ( Secs ): Start Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 12.00 1 Dwell (Secs) Coll Energy (eV) Cone V) 1 399.00 80.00 0.20 35 50 2 413.00 369.00 0.20 i0 i0 4 3 498.00 78.00 0.20 30 50 4 499.00 99.00 0.20 40 30 %,# Method Report Method Filer Last Modified: c:\masslynx\fluorochemicals.pro\acqudb\pfbs Friday, AuguSt 01, 2003 15:20:36 water Page 1 _mf Printed: Friday, August 01, 2003 15,29z16 _,I_ _ U HPII00 LC Pump Initial Conditions Solvents A% B% C% D% 90.0 I0.0 0.0 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar] Max Pressure (bar) Oven Temperature Left(oC) Oven Temperature Right(C) 0.300 20.0 0 400 35.0 35.0 HPIIO0 LC Pum_ Gradient Timetable The gradient Timetable contains 8 entries which are : Time 0.00 A% 90.0 B% i0.0 C% 00 D% Flow 0.0 0.300 Pressure 400 2.00 90.0 I0.0 00 0.0 0.300 400 5.00 10.0 90.0 00 0.0 0.300 400 _ 9.00 i0.0 90.0 00 0.0 0.300 400 9.50 0.0 i00.0 00 0.0 0.300 400 14.00 0.0 100.0 00 0.0 0.300 400 14.50 90.0 I0.0 00 0.0 0.300 400 20.00 90.0 I0.0 00 0.0 0.300 400 HPII00 LC Pump External Event Timetable The Timetable contains 6 entries which are : Time Initial 0.00 0.05 0.10 11.90 12.00 Column Switch Off Off Off Off Off Off Contactl Off On Off Off Off Off Contact2 Off O_f Off On Off Off HPII00 Autosampler Initial Draw Speed Eject Speed (#i/min) Draw Position (mm) Stop Time (mins) Injection Volume(#l) Vial Number Conditions 200.0 200 0.50 20.00 15.0 69 Contact3 Off Off Off Off On Off "" Contact4 Off Off Off Off Off Off V _ Tuning Method Report Method: C: \MASSLYNX\FLUOROCHEMICALS. Printed: Fri Aug 01 15:29:30 2003 PRO\ACQUDBkFLUOROCHEMS _ _I0, I0_ --T | I, Page 1 Dau 395.00 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture I Hexapole 2 Source Block Desolvation Temp. Temp. Pressures Analyser Gas Cell Vacuum Set 3.00 20 0.0 0.0 0.0 i00 300 Rdbk -2.93 -33 !00 299 Rdbk OFF 3.3e-3 Analyser LM Res 1 HM Res I IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas Flows Cone Gas Desolvation V Set 14.0 14.0 1.0 -2 15 2 14.0 14.0 2.0 650 Rdbk Rdbk 36 19 40 -64B 131.8 751.3 Quantify Calibration Report _ Study No.:L34910, Set No.z080103A, Ext.Date:08/01/03, Analyst:K.Risha Calibration: Last modified- P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\CurveDB\080103A Sun Aug 03 07:26:03 2003 Compound I name:C8 Acid(PFOA) CoefficieonftDeterminatio0n.:988097 Calibraticounrve"300.076*x + 2344.75 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: l/x, Axis trans: None 3.16e5- Page 1 Decatur BC x i Response- 01 : .... 0.0 I .... ' .... 200.0 } .... ' 'I I I l 400.0 I .... I .... 600.0 [ ' 'l' ] ] .... 800.0 Exygen Research, 3058 Research Drive, State College, PA 16801 I .... ing/L 1000.0 Quantify Calibration Report Study No.:L34910, Set No.:080103A, Ext.Datez08/01/03, Analyst:K.Risha Calibration: Last modified: Printed: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\080103A Sun Aug 03 07=26:03 2003 Sun Aug 03 07:32:22 2003 Compound2 name: C6 Sulfonate (PFHS) Coefficientof Determination:0.995587 Calibration curve: 57.3138 * x + 476.906 Response type: External Std, Area Curve type: Linear, Origin: Exclude,Weighting: l/x, Axistrans: None 5.83e4- Page 2 Decatur BC x x Response- 0 .,,, 0.0 _ .... _ .... 200.0 , . ,-". , i .... 400.0 , .... _ .... 600.0 _ .... _ .... 800.0 ,. ,.., _ng/L 1000.0 &_/gen Research, 3058 Research Drive, State College, PA 16801 Quantify Calibration Report %_ Study No.:L34910, Set No.:080103A, Ext.Date:08101/03, AnalystzK.Risha Calibration: Last modified: Printed: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\CurveDB\080103A Sttn Aug 03 07:26z03 2003 Sun Aug 03 07:32:22 2003 Compound3 name: C8 Sulfonate (PFOS) Coefficientof Determination:0.990916 Calibration curve: 35.0593 * x + 208.543 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: l/x, Axis trans: None Page 3 Decatur BC x x V 0.0 200.0 400.0 600.0 Exygen Research, 3058 Research Drive, State College, PA 16801 800.0 IIII I Quantify Calibration Report _ Study No.:L34910, Set No. z080103A, Ext.Date:08101/03, Analyst:K.Risha Calibration: Last modified: Printed: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\080103A Sun Aug 03 07_26:03 2003 Sun Aug 03 07:32:22 2003 Compound4 name: PFOSA Coefficient of Determination:0.996863 Calibration curve: 135.358* x + 849.062 Response type: External Std, Area Curve type: Linear, Origin: Exclude,Weighting: l/x, Axis trans: None 1.38e5- ' Page 4 Decatur BC x X Response V O- ,,., 0.0 =,-,,. ,',, _,, .",,. _ .... 200.0 400.0 _ .... _", ,"',, 600.0 .... ', ' ' '" , .... ',ng/L 800.0 1000.0 Exygen Research, 3058 Research Drive, State College, PA 16801 I i , , Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 1 Sample List: Last modified: Method: Last modified: Job Code : P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MetlLDB\Decatur Sun Aug 03 07:11:59 2003 iI, l_la_l Decatur BC BC 080103 Printed: Sun Aug 03 07:32:25 2003 Run# _o_A-2_o_ To O_OlOBA--_oT_) Name: 080103A-2001 Text : 1:C8 Acid (PFOA) XC072503-0, 0 ngJL Standard 080103A-2001 Sm (Mn, 2x3) 02-Aug-2003 02:27:16 LC/MS/MS #6 MRM of 4 ChannelsES- 2.00e4 110-_ j/_ 413 > 369 Area i ................ 2.00 _ __. -, , ,,, _ .... 4.00 6.00 ,.. ,'. ,', .,,,,. 8.00 , , , .... 10.00 ,, '.',. ,Time 12.00 2:C6 Sulfonate (PFHS) XC072503-0, 0 ng/t Standard 080103A-2001 Sm (Mn, 2x3) t 00_ #.0.24/0.90 4.74 02-Aug-2003 02:27:16 LC/MS/MS #6 I MRM of 4 ChannelsES- ,/_J/ 399 > 80 2.00 4.00 3:C8 Sulfona_e (PFOS) XC072503-0, 0 ng/L Standard 080103A-2001 Sm (Mn, 2x3) ,=^U^ 1"26 0 90A Time 6.00 8.00 10.00 12.00 02-Aug-2003 02:27:16 I LC/MS/MS #6 ,[/ MRM of 4 ChannelsES- _' ,_,.oQ_o, 499 > 99 6.63 9#1 / 11.3611.75 962 0" ' ' ' ' I .... I '" 2.00 ' ' I .... I .... 4.00 '1" ' ' ' ' I'" .... 6.00 , "" ....... , 8.00 , ' ' ' , ' ' ' ' , ' ' ' ' ,Time 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report t_ Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\San_leDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslym_\Fluorochemlcals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 2 Decatur BC BC 080103 Name: 080103A-2001 Text : 4 : PFOSA XC072503-0, 0 ng/L Standard _02-Aug-2003 02:27:16 _/ LC/MS/MS #6 080103A-2001 Sm (Mn, 2x3) MRM of 4 ChannelsES- 9.79 498 > 78 100"_ L 68 -t 0.s9-083;64 ,,,__a.2a_.40,a92_s,.ll 6.s1679 ...... 8.9a _ 10.64 11_8_6 i 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify San_le Report ,_ Study No.:L34910, Set No.:080103A, Ext.Date:08101103, Analyst:K.Ri=ha Sample List: Last modified: Method: Last modified: Job Code: P:_Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103A Stun Aug 03 07:25=44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 3 Decatur BC BC 080103 Name: 080103A-2002 Text : I: C8 Acid (PFOA) i !XC072503-1, 25 ng/h Standard 080103A-2002 Sm (Mn, 2x3) ,,,, 02-Aug-2003 02:49:0_= LC/MS/MS #E MRM of 4 ChannelsES- 9.13 413 > 369 Area i , ........... 2.00 _ . , .- _-.... 4.00 T, , ,_ 6.00 _, 2:C6 Sulfonate (PFHS) XC072503-1, 25 ng/L Standard 080103A-2002 Sm (Mn, 2x31 1q_O-_ , , , , ; , , :-L , . , ,-_ ,--7":-,_, ,Time 8.00 10.00 12.00 8.91 1572" 02-Aug-2003 02:49:05 LC/MS/MS #6 MRM of 4 ChannelsES399 > 80 9.29e3 Area ..... ,.... ,.... ','' ' ' ,' ''" 2.00 4.00 3:C8 Sulfonate (PFOS) XC072503-1, 25 ng/L Standard i .... _ .... 6.00 080103A-2002 Sm (Mn, 2x3) . . I _,,__ ,.... _ ........ ,.... 8.00 10.00 , .... ,Time 12.00 02-Aug-2003 02:49:05 LC/MS/MS #61 MRM of 4 ChannelsES- 9.26 499 99 ........ , .... 2.00 _ .... , .... 4.00 , .... ,......, 6.00 Olq _ _ .... , .... 8.00 , .... , .... 10.00 Area ,..., ,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 1_mf Quantify Sample Study No.:L34910, Report Set No.:080103A, Ext.Date:08/01/03, Analyst=K.Risha Sample List: Last modified= Method: Last modified: Job Code= P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 4 Decatur BC BC 080103 Name: 080103A-2002 Text : 4 : PFOSA XC072503-1, 25 ng/L Standard 080103A-2002 Sm (Mn,2x3) 02-Aug-2003 02:49:0. = LC/MS/MS #e MRM of 4 ChannelsES- 9.90 498 > 78 0 L, , , _ .... , .... 2.00 , .... ,,, _',, ,, ,_ , ,"," l" '' ' , .... 4.00 6.00 8.00 , '_-_', ' '_ ' i ;' ;' ,Time 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Re_ort _ Study No.:L34910, Set No.:080103A, Ext.Date:08101103, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\Sam_leDB\080103A Sun Aug 03 07:25:44 2005 P:\Data\LCMSMS6\Masslynx\Fluoroohemicals.PRO\MethDB\Decatur Sun Aug 03 07:ii:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 5 Decatur BC BC 080103 Name: 080103A-2003 Text : i: C8 Acid (PFOA) XC072503-2, 50 ng/h Standard 080103A-2003 Sm (Mn, 2x3) ot 100_ 9.13 17917- 02-Aug-2003 03:10:44 LC/MS/MS #6 MRM of 4 ChannelsES413 > 369 1.1le5 Area ! L Yl1- . .... , .... , .... ,, ,-_,,,,.,.,, ,, .... "l ..... l.., T;,, _,.,_,,,Time 2.00 4.00 6.00 8.00 10.00 12.00 %_ 2:C6 Sulfonate (PFHS) 'XC072503-2,50 n_L Standard 080103A-2003 Sm (Mn, 2x3) 02-Aug-2003 03:10:44 LC/MS/MS #6 MRM of 4 ChannelsES- 8.98 399 > 80 ll0/0l'_ . . ._ ,w, , , .... 2.00 i , ,', , , .... 4.00 3:C8 Sulfonate (PFOS) XC072503-2, 50 ng/L Standard 080103A-2003 Sm (Mn, 2x3) 10C_ % J .... i _ . . ,'t ,',, , , ..3..699_, .... , , ._.. ,-... r32T.i2m8ee4Area 6.00 8.00 10.00 12.00 02-Aug-2003 03:10:44 LCIMS/MS #6 MRM of 4 ChannelsES- 9.24 499 > 99 Area lid 2.00 4.00 6.00 8.00 _1.28e4 10.00 12.0T0ime , I , .... , ,' T,, ',' I ,', , , .... , .... , .... , .... , I r'',, I .... , .... ', Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify San_le Report _ Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\FluorochemicalsoPRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 6 Decatur BC BC 080103 Name: Text: 080103A-2003 4: PFOSA XC072503-2, 50 n_L Standard 080103A-2003 Sm (Mn, 2x3) In r 02-Aug-2003 03:10:44 LC/MS/MS #6 MRM of 4 ChannelsES- 9.90_ 7728 498 > 78 4.01e4 Area C,, ,, _ ,, ,, i .... _ .... _,, r, , _., ,,, _-_, ,. _ .... _ .... '_ ,' ...... 2.00 4.00 6.00 8.00 10.00 _,, ,_ _Time 12.00 lid Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %_ Study No.:L34910, Set No.:080103A, Ext.Date:08101103, Analyst=K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\Sam_leDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 7 Decatur BC BC 080103 Name: 080103A-2004 Text : i: C8 Acid (PFOA) XC072503-3, 100 ng/t Standard 080103A-2004 Sm (Mn, 2x3) 1 0_ 02-Aug-2003 03:32:27 LC/MS/MS #6 MRM of 4 ChannelsES- 9.13 413 > 369 34827- 2.10e5 Area j "''' '-_"_''' F'"' ' ' I .... ,' '"' _ .... , .... 2.00 4.00 6.00 _IulV 2:C6 Sulfonate (PFHS) XC072503-3, 100 ng/L. Standard 080103A-2004 Sm (Mn,2x3) f' "_" I ....... 8.00 8.98 C .... 10.00 ,'' "" ,Time 12.00 02-Aug-2003 03:32:27 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 'ZI 1i_ .... '_ '"' ' ' _ .... 2.00 i .... I '"r' 4.00 3:C8 Sulfonate (PFOS) XC072503-3, 100 ng/L Standard , I .... I .... 6.00 080103A-2004 Sm (Mn, 2x3) " 64811 3.94e4Area i .... I ' ' _' i ' ,'.-'_-i ' ' '-' ," ' ' ' _Time 8.00 10.00 12.00 02-Aug-2003 03:32:27 LC/MS/MS #6 MRM of 4 ChannelsES- 9.24 499 > 99 1i0_ 37011 2.21Areae4 iI, . , ,"T-r_. ,,-, , . ,, ,.i ,-.1 j . , .1. , .... , , , ,", , ,'_ , , i -_-, _ .... _ , , .-,-_', , ,-, ,Time 2.00 4.00 6.00 8.00 10.00 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 j i Quantify sample Report _ Study No.:L34910, Set No.:080103A, Ext.Date:08/01103, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11;59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 8 Decatur BC BC 080103 Name: 080103A-2004 Text : 4 : PFOSA XC072503-3, 100 ng/l. Standard 080103A-2004 Sm (Mn, 2x3) 1i0-_ 02-Aug-2003 03:32:2"; LC/MS/MS #_ MRM of 4 Channels ES- 9.90 498 > 78 7.93e4J 15082- Area = .... r .... _ .... _ .... J .... L .... , .... ", .... , .... _ ...... ',, ...'. t Time 2.00 4.00 6.00 8.00 0.00 12.00 V Ex1_en Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No. z080103A, Ext.Date:08101103, Analyst=K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Da_a\LCMSMS6\Masslynx\_luorochemicals.PR0\Sam_leDB\080103A Sun Aug 03 97:25:_4 2003 P:kData\LCMSMS6\MasslynxkFluorochemicals.PROkMethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 9 Decatur BC BC 080103 Name: 080103A-2005 Text : i: C8 Acid (PFOA) XC072503-4, 250 ng/L Standard 080103A-2005 Sm (Mn, 2x3) 100 02-Aug-2003 03:54:13] 9.13 78794- LC/iVlS/MS #_ MRM of 4 Channels ES- I 413 > 369] 4.78e5 Area j C .... ',_:_',' r_..-, 2.00 _, '-,-, , .... 4.00 2:C6 Sulfonate (PFHS) XC072503-4, 250 ng/h Standard 080103A-2005 Sm (Mn, 2x3) , .... , .... 6.00 ,.... i .... 8.00 JL i ,,, ,',, ,,, 10.00 .... ,Time 12.00 02-Aug-2003 03:54:13 LC/MS/MS#6 MRM of 4 ChannelsES- 8.98 399 > 80 1i_ ? ' ' ' I .... I ' [I ' '1 _ l' 2.00 I ' ' ' .... 4.00 3:C8 Sulfonate (PFOS) XC072503-4, 250 ng/L Standard 080103A-2005 Sm (Mn, 2x31 _ .... I .... 6.00 157701 I .... _ .... ' .... _ .... 8.00 10.00 9.57e4Area l .... ,Time 12.00 02-Aug-2003 03:54:13 LC/MS/MS #6 MRM of 4 ChannelsES- 9.24 499 > 99 2.00 4.00 6.00 8.00 10.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 12.00 Quantify Sample Report _ Study No.:L34910, Set No.:080103A, Ext.Date:08101103, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P_\Data\LCMSMS6\Maaslynx\FluorochemicalsPRO\Sam_leDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicala.PRO\MethDB\Decatur Su_ Aug 03 07:11:59 2003 Printed: Sun Aug 03 07_32:25 2003 Page I0 Decatur BC BC 080103 Name: 080103A-2005 Text : 4 : PFOSA XC072503-4, 250 n_L Standard 080103A-2005 Sm (Mn, 2x3) 02-Aug-2003 03:54:1_ LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 111_ 36693- 1.95e5Area I_ 0'. ,,., .... ,,,.. _ .... _ .... ,,', , Y .... t .... , .... , ...... _ _ .... ,Time 2.00 4.00 6.00 8.00 0.00 12.00 I14 Exygen Research, 3058 Research Drive, State College, PA 16801 %q_# Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:kData\LCMSMS6kMaSslynx\Fluorochemicals.PROkSam_leDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur S_n Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page ii Decatur BC BC 080103 Nsune : 080103A-2006 Text : i: C8 Acid (PFOA) XC072503-5, 500 ng/L Standard 080103A-2006Sm (Mn, 2x3) 1_,_ 02-Aug-2003 04:15:54 LC/MS/MS #6 9.12 171634- MRM of 4 ChannelsES413 > 369 1.0le6 Are_ _ /i1' '' _'_"', .... 2.00 i .... _ .... 4.00 2:C6 Sulfonate (9FHS) XC072503-5, 500 ng/L Standard 080103A-2006Sm (Mn, 2x3) i .... i' ' "' _'"' ' _ .... 6.00 8.00 i<, . . . _ .... 10.00 _ ..... i Time 12.00 02-Aug-2003 04:15:54 LC/MS/MS #6 MRM of 4 ChannelsES- 8.98 399 > 80 1i/! .... ', .... , .... 2.00 , .... i .... 4.00 3:C8 Sulfonar.e (gFOS) XC072503-5, 500 ng/L Standard 080103A-2006 Sm (Mn, 2x3) , .... i .... 6.00 , .... ,3..1.2. 811i, ,', ,', ,"', ,', , .... "71T.9im0ee5Area 8.00 10.00 12.00 19171 02-Aug-2003 04:15:54 LC/MS/MS #6 MRM of 4 ChannelsES- 1.1le5 Area 11o/i (3' .... llW i ,',, ,t .... 2.00 _ .... i .... 4.00 _ .... _ .... 6.00 9.24 1 499 > 99 _ .... , .... , .... i ,, ,', i .... 1Time 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Re_ort Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P=\Data\LCMSMS6\Masslynx\Flucrcchemicals.PRO\Sam_leDB\080103A Sun Aug 03 07=25=44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 12 Decatur BC BC 080103 Name: 080103A-2006 Text : 4 PFOSA XC072503-5, 500 ng/L Standard 080103A-2006 Sm (Mn, 2x3) 02-Aug-2003 04:15:54( LC/MS/MS #6 I MRM of 4 ChannelsES- I 9.92 _ 498 > 78I 1i0_ 72894 3.82e5Area _4 .... _'..., .... _ .... , .... , .... , .... , .... ,.,,,, 2.00 4.00 6.00 8.00 I ....... 10.00 , .... i Time 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 i |I I Quantify sample Report _ Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Page 13 Sample List: Last modified: Method Last modified: Job Code : P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\Sam_leDB\080103A Sun Aug 03 07:25:44 2003 P: \Data\LCMSMS 6 \Mass lynxkFluorochemical s. PRO\MethDB Sun Aug 03 07:11:59 2003 \Decatur Decatur BC BC 080103 Printed: Sun Aug 03 07:32:25 2003 Name: 080103A-2007 Text : I: C8 Acid (PFOA) XC072503-6, 1000 ng/L Standard 080103A-2007Sm (Mn, 2x3) 02-Aug-2003 04:37:34 LC/MS/MS #E MRM of 4 ChannelsES- 9.13 413 > 369i 1%1_0_ 315768- .. 1.84e6Area !J 0' .... , ,-, . . , .... , .... , .... ,'. ,. , , .... ,'.",', . , ....... i .... , .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 %_#' 2:C6 Sulfonate (PFHS) XC072503-6, 1000 ng/L Standard 080103A-2007 Sm (Mn, 2x3) 02-Aug-2003 04:37:34 LC/MS/MS #6 MRM of 4 ChannelsES- 8.98 399 > 80 11/l O r .... J .... i .... 2.00 J .... , .... 4.00 3:C8 Sulfonate (PFOS) XC072503-6, 1000 ng/h Standard 080103A-2007 Srn (Mn, 2x3) i .... , .... 6.00 58308_ , .... , .... i . . .". i ..... 8.00 10.00 3.49e5Area , .... ,Time 12.00 02-Aug-2003 04:37:34 LC/MS/MS #6 MRM of 4 ChannelsES- 9.25 499 > 99 Area Ili,0 I, .., .... , .... 2.00 , .... , .... 4.00 , .... , .... 6.00 , .... _ .... 8.00 J .... i...., 10.00 .... _Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _F Study No.:L34910, Set No.=080103A, Ext.Date:08/01/03, Analyst=K.Risha Sample List: Last modified: Method: Last modified: Job Code: P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103A Sun Aug 03 07=25=44 2003 P_\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\MethJ3B\Decatur Sun Aug 03 07:11=59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 14 Decatur BC BC 080103 Name: 080103A-2007 Text : 4 : PFOSA XC072503-6, 1000 n_L Standard 080103A-2007Sm (Mn, 2x3) 10C 02-Aug-2003 04:37:34 LC/MS/MS #6 MRM of 4 ChannelsES- 9.92 _ 137821 498 > 78 7.22e5 1 Area ! C '''' _ .... i .... 2.00 J .... i .... 4.00 i .... I .... 6.00 i .... i .... 8.00 Ji i ....... 0.00 i '"'' iTime 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Re_ort Study No.:L34910, _fw Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Deoatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07=32:25 2003 Page 15 Decatur BC BC 080103 Name: 080103A-2008 Text : i: C8 Acid (PFOA) Methanol Wash . 080103A-2008 Sm (Mn, 2x3) 10C /= 02-Aug-2003 04:59:21 LC/MS/MS #6 MRM of 4 ChannelsES- 9.15 413 > 36 5.39e3 Area 0 ''' ' I .... , .... 2.00 , .... I .... 4.00 , .... , .... 6.00 I .... _ .... 8.00 , .... , .... 10.00 ,,,,. ,Time 12.00 _ 2:C6 Sulfonate (PFHS) Methanol Wash 080103A-2008 Sm (Mn, 2x3) 10t-(_'"_.16 -IA081 120 289 . ..... .,_oo 4.80_./../ 620^-- - 02-Aug-2003 04:59:21 _/ MRM of 4LCh/MaSnn/MeSlsES#6- 8.96 399 > 80 "[\ 9 55 1022 10.62 775 8.108.671 \ _ _" / 11:80 2.00 4.00 6.00 8.00 10.00 12.00 3:C8 SulfonaCe Methanol Wash (PFOS) 060103A-2008 Sm (Mn, 2x3) 1 02-Aug-2003 04:59:21 I LC/MS/MS #6 ,I/ MRM of 4 ChannelsES- V93o 10. 11.34699>8 2.00 4.00 6.00 8.00 10.00 %J _en Research, 3058 Research Drive, State College, PA 16801 12.00 Quantify Sample Report ,,_. Study NO.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst=K.Risha San_le List: Last modified: Method: Last modified: Job Code: P:\Data\LC_gMS6\Maeslynx\Fluoroohemicals.PRO\San_leDB\080103A Sun Aug 03 07:25:44 2003 P=\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\MethDB\Decatur Sun AUg 03 07:11:59 2003 Printed: Sun Aug 03 07=32:25 2003 Page 16 Decatur BC BC 080103 Name= 080103A-2008 Text : 4 : PFOSA Methanol Wash 080103A-2008 Srn(Mn, 2x3) 100-_ 0 13 -]'_" 4 === 3.54 4.02 0_,-Aug-2003 04:59:21 LC/MS/MS #6 MRM of 4 ChannelsES- 9.93 498 78 A 881 7.67 8.84 _,.,, II 10.53 11.12 ! 2.00 4.00 6.00 8.00 10.00 12.00 I_,,# Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:080103A, Ext.Da_e:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\San_leDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6kMasslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 17 Decatur BC BC 080103 Name: 080103A-2009 Text : i: C8 Acid (PFOA) Reagent Blank 080103A-2009Sm (Mn, 2x3) lnO,-_ 02-Aug-2003 05:20:57 LC/MS/MS #E MRM of 4 ChannelsES413 > 3691 1.71e4 Area ...... ,.'... j .... _,,,'. j'. ,,,', .... ,.... ,.... , .... ,.... , .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 _ 2:C6 Sulfonate (PFHS) Reagent Blank 02-Aug-2003 05:20:57 I LC/MS/MS #6 080103A-2009S1.m49(Mn, 2x3) 100-j 0.13070 A 224 268 397 . _ 7.1.17.53 87R 8.95 9M9R9M of 4 Chan3n9e9ls>ES8-0=_ _- P10.26 11.41 =34 ....... 3.49 o=.1 5.08 5.886.77 _'" _,__ /i1 .',.... , , , i , , , ,"] r , , , i , , , ,'1 , , , i , , , , i , , , , i , , ,', i , , , , i , , , , i , , , , i .... 2.00 4.00 6.00 8.00 10.00 i m|me" 12.00 3:C8 Sulfonate Reagent Blank (PFOS) 02-Aug-2003 05:20:57 080103A-2009Sm (Mn, 2x3) 10C 1.04 A % 0.46 1.81 280 3.183.69 4.43 5.29 5.966.48 _/ MRM of 4LCC/hMaSn/nMeSlsES#E- 9 27 11.38499 > 99! "A 1109 A 1.03e3 716 86 91// 1016 7.62 8.33 " (_ .... _ .... , .... 2.00 _ .... , .... 4.00 , .... , .... 6.00 ,,,.. ,',..., 8.00 .... , .... , .... ,Time 10.00 12.00 ExyDen Research, 3058 Research Drive, State College, PA 16801 qlmf Quantify Sa_le Report Study No.:L34910, Set No.:080103A, Ext.Date_08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Maesly_x\Fluorocheanicals.PRO\Sam_leDB\080103A S_n Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals. PRO\MethDB\Decatur Sun Aug 03 07:11:59 2005 Printed: Sun Aug 03 07:32:25 2003 Page 18 Decatur BC BC 080103 Name: 080103A-2009 Text : 4 : PFOSA Reagent Blank 080103A-2009Sm (Mn,2x3) _-Aug-2003 05:20:57 _/ LC/MS/MS #6 MRMof4 ChannelsES- 9.93 498 > 78 Time 2.00 4.00 6.00 8.00 10.00 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify san_le Report %_I Study No.:L34910, Set No.:080103A, Ext.Date:08101103, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Coda: P:\DatakLCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103A Sun Aug 03 07:25:44 2003 Pz\Data\LCMSMS6\Masslynx\FluorochemIcals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 19 Decatur BC BC 080103 Name: 080103A-2010 Text : i: C8 Acid (PFOA) Reagent Spk A, 50 ng/L 080103A-2010Sm (Mn, 2x3) 1,_n_ 02-Aug-2003 05:42:42 LC/MS/MS #6 9.13 18939- MRM of4 ChannelsES- 413 > 369 1.12e5 Area | i1 J, .... ' ' ' I ' ' ' ' I '--' ' ' I'' ' ' ' I ' ' ' ' _ '" ' " I '" ' ' _ ' ' ' " 2.00 4.00 6.00 8.00 ' ' '-' I '_'_' ' ' 1 ,_, , I Time 10.00 12.00 %_/ 2:C6 Sulfonate (PFHS) Reagent Spk A, 50 ng/h 080103A-2010 Sm (Mn, 2x3) il0_7",, ,-, i .... , .... 2.00 , .... _ , _-, ; _ _ ,--, , .... 4.00 6.00 3:C8 Sulfonate (PFOS) Reagent Spk A, 50 ng/h 080103A-2010 Sm (Mn, 2x3) 8.96 _-, _ ' i , ,_ 8.00 , .... 02-Aug-2003 05:42:42 LC/MS/MS #6 MRM of4 ChannelsES399 > 80 e , , =_ , ,-,'_-_Time 10.00 12.00 02-Aug-2003 05:42:42 LC/MS/MS #6 MRM of 4 ChannelsES- 9.25 499 > 99 1 re 1(i[/1__ , ', , , ,', , " t"' 2,0T11]._..,......... 2.00 4.00 8.00 8.00 10.00 a-l,ii2ei41 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103A, Ext.Date:08/01/03, AnalystsK.Risha Sample List: Last modified: Method= Last modified= Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103A Sun Aug 03 07:25=44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\MethDB\Decatur Sun Aug 03 07=11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 20 Decatur BC BC 080103 Name: 080103A-2010 Text : : PFOSA Reagent Spk A, 50 ng/L 080103A-2010Sm (Mn, 2x3) 10 02-Aug-2003 05:42:42 LC/MS/MS #6 MRM of 4 ChannelsES- 675 3.52e4 Area_ i 0 I .... ,.,,',, :.-,", ,,,,',, _',,,, 2.00 4.00 .... , ,', ,",, .... ,.',.. 6.00 8.00 ,-, r,, ,,,."., 10.00 .... ,Time 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample ReDort _ Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Rilha Page 21 Sample List: Last modified: Method: Last modified: Job Code : P:\DatakLCMSMS6\MasilynxkFluorochemicals.PRO\SampleDB\080103A Sun Aug 03 07:25:44 2003 P: \Data\LCNSMS 6 \Nas s ly_x\Fluor0chemicals. PR0\MethDB\Decatur Sun Aug 03 07:11:59 2003 Decatur BC BC 080 i03 Printed: Su_ Aug 03 07:32:25 2003 Name: 080103A-2011 Text : I: C8 Acid (PFOA) Reagent Spk B, 500 ng/L 080103A-2011 Sm (Mn, 2x3) 1(P07 0 E.... I .... I .... 2.00 _ .... _ .... 4.00 2:C6 Sulfonate (PFHS) Reagent Spk B, 500 ng/L 080103A-2011 Sm (Mn, 2x3) (li0 I .... , .... , .... 2.00 , .... i .... 4.00 3:C8 Sulfonate (PFOS) Reagent Spk B, 500 ng/L 080103A-2011 Sm (Mn, 2x3) _'" '",, .... 6.00 J .... , .... 6.00 02-Aug-2003 06:04:2_ LC/MS/MS #E MRM of 4 ChannelsES-i 9.15 413 > 369 163063- 9.90e5 Area _ -I _ .... i .... 8.00 L '_ ,'' _ .... 10.00 i .... _Time 12.00 02-Aug-2003 06:04:23 LC/MS/MS #6 MRM of 4 ChannelsES- 8.99 399 > 80 4 .... , .... 8.00 1t ' ' ' '_ .... 10.00 ere ,' ,"'' iTime 12.00 02-Aug-2003 06:04:23 LC/MS/MS #6 MRM of4 Channels ES- 9.25 499 > 99 Area 110-_ i1,., . .... , .... 2.00 r", ,',,,..",.,,. 4.00 V ,-,, .... 6.00 175831 , .... t .... , .... ,-...,_ 8.00 10.00 1.05e5 .... zTime 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08101/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Massllrnx\Flu0rochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 22 Decatur BC BC 080103 Name: 080103A-2011 Text : 4 : PFOSA Reagent Spk B, 500 ng/L 02-Aug-2003 06:04:23 LC/MS/MS #6 080103A-2011Sm (Mn,2x3) MRMof 4 ChannelsES- 9.89 498 > 78 lq0--_ 65424- 3.52e5 1 Area i ,L 0',,,, _ .... _ .... _,,,, ,',,,, _,',,,, .... _'"'L .... ,''' , ,',,_ .... _Time 2.00 4.00 6.00 8.00 10.00 12,00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify sample Report q,_ Study No.:L34910, Sat No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\Sam_leDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PROkMethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 23 Decatur BC BC 080103 Name: 080103A-2012 Text : 1:C8 Acid (PFOA) XC072503-I, 25 n_L Standard " :" 02-Aug-2003 06:26:1C LC/MS/MS #6 080103A-2012 Sm (Mn, 2x3) MRM of 4 ChannelsES- 1"" " _ ^^_^-9"14 - _'u 413 > 369 5.69e4 Are_ i ....... _, ',_ , , ,', ,' ,-", ' ,'T_ ,_,, -,'-, ._.Tr, ' , ' _ ................ 2.00 4.00 6.00 8.00 10.00 ,Time 12.00 _ 2:C6 Sulfonate (PFHS) XC072503-1, 25 ng/L Standard 080103A-2012 Sm (Mn, 2x3) 02-Aug-2003 06:26:10 LC/MS/MS #6 MRM of 4 ChannelsES-' 8.99 399 80i i/10__1 _- ,' i .... 2.00 I .... , .... 4.00 , .... I .... 6.00 J .... ]l 8.00 iiia . 10.00 12.00 3:C8 Sulfonate (PFOS) XC072503-1, 25 ng/L Standard 080103A-2012 Sm (Mn, 2x3) 02-Aug-2003 06:26:10_ LC/MS/MS #6I MRM of 4 Channels ES- I 9.25 499 > 99I ..., , ,., ,,,, ,. , ,,,, , , , , , ,,,, , 2.00 4.00 6.00 8.00 11J 10.00 Exygen Research, 3058 Research Drive, State Collage, PA 16801 Areal T 12.00 Quantify Sample Report %_ Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx_Fluorochemicale.PRO\SampleDB\080103A S_n Aug 03 07:25:44 2003 Pz\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 24 Decatur BC BC 080103 Name: 080103A-2012 Text : 4 : PFOSA XC072503-1, 25 ng/L Standard 080103A-2012 Sm (Mn, 2x3) 02-Aug-2003 06:26:1( LC/MS/MS #e MRM of 4 ChannelsES- 9.88 498 > 78i I Area ! ......."... I i _, i ,--'_, t ' ' ' " '1 ' ' '"" 2.00 4.00 ] .... I ' " ' "_1 " ' ' ' I ' ' 6.00 8.00 I r. ......I. ' _'"1 10.00 ; , Time. 12.00 V Ex1_en Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha San_le List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Massllrnx\Fluorochemicals.PRO\Sam_leDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32=25 2003 Page 25 Decatur BC BC 080103 Name: 080103A-2013 Text : i: C8 Acid (PFOA) 534910-5 Spk C, 5000 rig/L, DF=10 080103A-2013 Sm (Mn, 2x3) 02-Aug-2003 06:47:56_ LC/MS/MS #6I MRM of 4 Channels ES-i 9.13 413 > 369 9.32e5i Area | t ! 11o/1 0[ ' ' _ ' fi-_" 2.C)0 '' '"' 15797111 4.00 6.0(3 8.()0 ' I ' ' ' ''' ' t' ' " ''' I' '' I' 10.00 1'2'.0_me ' ' I ' ' ' ' I' ' ' ' " I 2:C6 Sulfonate (PFHS) 534910-5 Spk C, 5000 ng/L, DF=10 080103A-2013 Sm (Mn, 2x3) 02-Aug-2003 06:47:56 LC/MS/MS #6 MRM of 4 Channels ES- 8.98 399 > 80 0 ''t .... _ .... i .... 2.00 _"' ' ' ' i .... 4.00 3:C8 Sulfonate (PFOS) L34910-5 Spk C, 5000 ng/L, DF=10 080103A-2013 Sm (Mn, 2x3) i .... _ .... 6.00 ', .... ,' '"'' 8.00 I .... _ .... 10.00 , .... _Time 12.00 02-Aug-2003 06:47:56 LC/MS/MS #6 MRM of 4 Channels ES- 9.25 499 > 99 Area lilW' 0 _, ,-, ,-T".... , .... 2.00 , .... , .... 4.00 , .... , .... 6.00 , .... _ .... 8.00 , .... _.", , ' L .... kTime 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L3&910, Report Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha San_le List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\San_leDB\080103A Sun Aug 03 07:25:44 2003 Pz\Da_a\LCMSMS6\Massly_x\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 26 Decatur BC BC 080103 Name: 080103A-2013 Text : 4 : PFOSA L34910-5 Spk C, 5000 ng/h,DF=10 080103A-2013 Sm (Mn, 2x3) 02-Aug-2003 06:47:5E LC/MS/MS #E MRM of 4 ChannelsES- 9.90 498 > 78 1(o/1 79517- 4.1A8rea5 __ 0 I .... _ .... ,, ',,,, 2.00 .... ,,,,, 4.00 J .... , .... 6.00 _ .... _ .... 8.00 , ....... 10.00 _ .... ,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha San_le List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Maselynx\Fluorochemicals.PROkSampleDBk080103A Su_ Aug 03 07:25=44 2003 P:\DatakLCMSMS6kMasslynx\Fluorochemicals.PROkMethDBkDecatur Stul Aug 03 07=ii=59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 27 Decatur BC BC 080103 Name: 080103A-2014 Text : I: C8 Acid (PFOA) L34910-I0 Spk D, 5000 n_t, DF=I0 080103A-2014Sm (Mn, 2x3) 02-Aug-2003 07:09:3=. LC/MS/MS #6 MRM of4 ChannelsES- ! I 10 1661 9.88e5 Area (3' . , , , _ , , , ,, , 2.00 I, , , , Ii , , , ,, , , , ,, , , , i 4.00 6.00 ' ' ' j , , , T I ' ' ' ' , ' ' ' ' l ' ' ' ' iTime 8.00 10.00 12.00 _ 2:C6 Sulfonate (PFHS) L34910-10 Spk D, 5000 ng/t, DF=10 080103A-2014Sm (Mn, 2x3) 1. 3219 02-Aug-2003 07:09:35 LC/MS/MS #6 MRM of 4 ChannelsES- 1.89e5 Area 0 r .... _ .... , .... 2.00 , .... , .... 4.00 3:C8 Sulfonate (PFOS) L34910-10 Spk D, 5000 ncj/L, DF=10 080103A-2014 Sm (Mn, 2x3) 1 _ .... , .... 6.00 , .... , .... 8.00 , .... ,', , , , , , , ,', _Time 10.00 12.00 2693 02-Aug-2003 07:09:35 LC/MS/MS #6 MRM of 4 ChannelsES- 1.62e5 Area _1 .... _ .,,, .... j .... , .... j .... , .... ,,,',',, .... _ .... , .... _..,.,Time 2.00 4.00 6.00 8.00 10.00 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %_ Study No.:L34910, Set No.:080103A, Ext.Date=08/01/03, Analyst:K.Risha Sample List: Last modified: Method= Last modified: Job Code: P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\Sam_leDB\080103ADecatur Sun Aug 03 07:25:44 2003 P=\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\MethDB\Decatur Sun Aug 03 07=11=59 2003 Printed: Sun Aug 03 07:32=25 2003 Page 28 BC BC 080103 Name= 080103A-2014 Text : 4 : 9FOSA L34910-10 Spk D, 5000 ng/L, DF=10 080103A-2014 Sm (Mn, 2x3) 02-Aug-2003 07:09:3.= LC/MS1MS #6 MRM of 4 Channels ES- 9.89 498 > 78 Are_ 0'_ .... _'_ ' ' ' _ .... r .... , ..."., .... , _ '"'., .... , '' '" i .... , .... I' . ,Time 2.00 4.00 6.00 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, StaLe College, PA 16801 Quantify Sample Report V Study No.:L34910, Set No.:080103A, Ext.Date:08/01103, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDR\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Su_ Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 29 Decatur BC BC 080103 Name: 080103A-2015 Text : I: C8 Acid (PFOA) L34910-11 Spk E, 5000 ng/L, DF-10 080103A-2015 Sm (Mn, 2x3) 02-Aug-2003 07:31:1; LC/MS/MS #E MRM of 4 ChannelsES- 9.13 413 > 369 Area ! 1 O' .... _->'''_''" 2.00 _"''' i .... 4.00 %I_ 2:C6 Sulfonate (PFHS) L34910-11 Spk E, 5000 ng/L, DF=10 080103A-2015 Sm (Mn, 2x3) 5"''' L.... 6.00 _ .... , .... 8.00 _ .... _ .... 10.00 I .... _Time 12.00 02-Aug-2003 07:31:17 LC/MS/MS #6 MRM of 4 ChannelsES- 8.96 399 > 80 Area 1i0_ 2.00 4.00 3:C8 Sulfonate (PFOS) L34910-11 Spk E, 5000 ng/L, DF=10 080103A-2015 Sm (Mn, 2x3) 6.00 323341 8.00 10.00 1.90e5 12.00 9.27 02-Aug-2003 07:31:17 LC/MS/MS #6 MRM of 4 Channels ES- 499 > 99 0 _.... , .... ..., .... 2.00 , .... , .... 4.00 , .... , .... 6.00 , .... , .... 8.00 , .... , .... 10.00 , .... ,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Re_ort Study No.:L34910, Set No.:080103A, Ext.Date:08101103, Analyst:K.Risha Sample List: Last modified: Method: Last modified_ Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Sun Aug 03 07:25z44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals. PR0\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed_ Sun Aug 03 07:32:25 2003 Page 30 Decatur-BC BC 080103 Name: 080103A-2015 Text : 4: PFOSA L34910-11 Spk E, 5000 ng/L, DF=10 080103A-2015 Sm (Mn, 2x3) 02-Aug-2003 07:31:17 LC/MS/MS #6 MRM of 4 ChannelsES- 9.88 498 > 78 Area | 0 _ ' "'' _ .... , '' ' ' , .... , ..... ,''' ', .... , .... ,'' ' . _ .... I .... _ .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 %,J V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: LaSt modified= Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 31 Decatur BC BC 080103 Name= 080103A-2016 Text : i: C8 Acid (PFOA) L34910-20 Spk F, 5000 ng/L, DF-10 080103A-2016 Sm (Mn, 2x3) 1(O7 02-Aug-2003 07:52:54( 9.13 179090- LC/MS/MS #6[ MRM of 4 Channels ES-i 413 > 369} 1.02e6 Area 4 t J o' ,., .... , .... _ .... , .... , .... , .... _ .... , .... JtL, , . j .... ,. ,.._Time 2.00 4.00 6.00 8.00 10.00 12.00 %_ 2:C6 Sulfonate (PFHS) L34910-20 Spk F, 5000 rig/L, DF=10 080103A-2016 Sm (Mn, 2x3) 02-Aug-2003 07:52:54 LC/MS/MS #6 MRM of 4 ChannelsES- 8.96 399 > 80 Area 1(o/l C _ .-,,., ...., .... 2.00 _ ,-.', . , .... 4.00 3:C8 Sulfonate (PFOS) L34910-20 Spk F, 5000 ng/t, DF=10 080103A-2016 Sm (Mn, 2x3) i .... _ .... 6.00 323431 , .... , .... , , ,.. , .... 8.00 10.00 1.91e5 -, .... ,Time 12.00 02-Aug-2003 07:52:54_ LC/MS/MS #6I MRM of 4 ChannelsES- I 9.25 499 > 99I Area 111 0', , ., .... ,,,.. 2.00 , .... , .... 4.00 , .... , .... 6.00 722481 4.13e5 , .... , .... , .... ,,., ,. , .... _Time 8.00 10.00 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample _14m_ StUdy No.:L34910, Report Set No.:080103A, Ext.Date:08/01/03, Analyat:K.Risha Sample List: Last modified= Method: Last modified: Job Code: P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\Saz_leDB\08G103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MathDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 32 Decatur BC BC 080103 Name: Text: 080103A-2016 4 : PFOSA L34910-20 Spk F, 5000 ng/L, DF=10 080103A-2016 Sm (Mn, 2x3) 02-Aug-2003 07:52:54 LC/MS/MS #6 MRM of 4 ChannelsES- 110 1006 5.19e5 Area _ ! 01.'..., .... i .... 2.00 J, ,.,, .... 4.00 , .... , .... 6.00 i .... 1.... 8.00 _-, ,-,, i .... 10.00 _. ,,, i Time 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify sample Report _mJ Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:kDatakLCMSMS6kMasslynx\Fluorochemicale.PROkSam_leDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 33 Decatur BC BC 080103 Name: 080103A-2017 Text : i: C8 Acid (PFOA) XC072503-2, 50 ng/L Standard 080103A-2017 Sm (Mn, 2x3) 02-Aug-2003 08:14:4i LC/MS/MS #6 MRM of 4 ChannelsES- 9.13 413 > 36! Are_ 0 '_'_' .... " ' , '' ' ' i_ ' ' ' , '_ ' ' _''' 2.00 4.00 ', .... 6.00 , ...',.. , _ .... ;.. ,_, ,., .-,Time 8.00 10.00 12.00 _1_# 2:C6 Sulfonar_e (PFHS) XC072503-2, 50 ng/L Standard 080103A-2017 Sm (Mn, 2x3) ,' ' ' ..... ............. 2.00 4.00 , ," ' ' " 6.00 8.98 '; "' _''' i .... 8.00 02-Aug-2003 08:14:41 LC/MS/MS#6 MRM of 4 ChannelsES399 > 80 .0 i .... i .... i Time 10.00 12.00 3:C8 Sulfonate (PFOS) XC072503-2, 50 ng/L Standard 02-Aug-2003 08:14:41 LC/MS/MS #6 080103A-2017 Sm (Mn, 2x3) MRM of 4 ChannelsES- 9.24 499 > 99 10C % (3 _,,,, V , , , , _ , ,,, ,,, , , c,",,, 2.00 4.00 , ,-,, , .... 6.00 2233] i ..... , .... 8.00 lJ, , ,_,,,, 10.00 1.34e4 Area , , , , Time 12.00 l I e Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %_ Study No.;L34910, Set No.=080103A, Ext.Date:08101103, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslymx\Fluorochemicals.PRO\SampleDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07=11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 34 Decatur BC BC 080103 Name: 080103A-2017 Text : 4 : PFOSA XC072503-2, 50 n_h Standard 080103A-2017 Sm (Mn, 2x3) lq0_ 02-Aug-2003 08:14:41 LC/MS/MS #6 MRM of 4 ChannelsES- 9.89 498 > 78 7957- 4.10e4 Area | 0,_-_,, ,, _ .... _ .... 2.00 _,,'_' ,'_,,,', 4.00 _,',,, _ .... 6.00 L, _,,-_ .... 8.00 _ ....... 10.00 _, ,',, _Time 12.00 '_WIr Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _/ Study NO.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst=K.Risha Sample List: Las_ modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Su_ Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 35 Decatur BC BC 080103 Name: 080103A-2018 Text : i: C8 Acid L34910-5 (PFOA) 080103A-2018 Sm (Mn, 2x3) 1CO7 9.15 115451- 02-Aug-2003 08:36:27 / LC/MS/MS #6( MRM of 4 ChannelsES413 > 369 6.67e5 Area " ''' _ .... _ .... 2.00 .tlqm_ 2:C6 Sulfonate L34910-5 (PF'HS) _ .... _ .... 4.00 080103A-2018 Sm (Mn, 2x3) _ .... _ .... 6.00 _ .... _ .... 8.00 , , ,, _ .... 10.00 _ .... _Time 12.00 02-Aug-2003 08:36:27 LC/MS/MS#6 MRM of 4 ChannelsES- 8.98 399 > 80 0 ''' " I .... , .... 2.00 j'.. . . , . . .". , _'... , ...'. 4.00 6.00 3:C8 Sulfonate L34910-5 (gFOS) 080103A-2018 Sm (Mn, 2x3) , .'. . _ .... 8.00 , .... , .... 10.00 j .... _Time 12.00 02-Aug-2003 08:36:27 LC/MS/MS #6 MRM of 4 ChannelsES- 9.27 499 > 99 111 .... , . .,. _ .... , .-... , .... , .... , .... = .... , ...6. 061,31.... , .... , .... 3_.T5im8ee5Area 2.00 4.00 6.00 8.00 10.00 12.00 V ExYgen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _f Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, AnalystzK.Risha Sample List: Last modified; Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur Sun Aug 03 07:11:5% 2003 Printed: S_n Aug 03 07:32:25 2003 Page 36 Decatur BC BC 080103 Name: 080103A-2018 Text : 4 : PFOSA L34910-5 080103A-2018Sm (Mn, 2x3) 100_ 02-Aug-2003 08:36:27 LC/MS/MS #6 MRM of 4 ChannelsES- 192.198082- 4968.287e85 Area | .... , .".,, J ..'., , .... _ .... , .... , .... , .... , .... , ...... , , .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 V Exygen Research, 3058 Research Drive, Stats College, PA 16801 Quantify sample Report _ Study No.:L34910, Set No.:080103A, Ext.Date:08101103, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Sun Aug 03 07:25:44 2003 Pz\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 37 Decatur BC BC 080103 Name: 080103A-2019 Text : i: C8 Acid (PFOA) L34910-5 Rep 080103A-2019 Sm (Mn, 2x3) 100-_ 9.13 82762- 02-Aug-2003 08:58:1 LC/MS/MS #6 MRM of4 ChannelsES413 > 369 4.8le5 Area I .... _ ,.. , .... 2.00 2:C6 Sulfonat:e L34910-5 Rep (PFHS) _.,,.. , .... 4.00 080103A-2019 Sm (Mn, 2x3) _ .... , .... 6.00 , .... _..' ..... 8.00 8.98 , .... 10.00 j .... ,Time 12.00 02-Aug-2003 08:58:12 LC/MS/MS #e MRM of 4 ChannelsES399 > 801 0L"''' _ ' ' :' i .... ,'''' i .... ,'''' i ' '' ' I .... J'''' 2.00 4.00 6.00 8.00 i ' ' ' ;,'' :-','' 10.00 '' bTime 12.00 3 : C8 Sulfonat:e (PFOS) iL34910-5 Rep I 080103A-2019 Sm (Mn, 2x3) 02-Aug-2003 08:58:12 LC/MS/MS #6 MRM of 4 ChannelsES- 9.25 499 > 99 Area i1 .... _, , ,.., _., .., _ .... _ .... 2.00 4.00 _ .... _ .... 6.00 _ .... _ ,, ,.. _ .... _ .... 8.00 10.00 _ .... _Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:080103A, Ext.Date:08101/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\San_leDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 38 Decatur BC BC 080103 Name: Text: 080103A-2019 4: PFOSA L34910-5 Rep 080103A-2019 Sm (Mn, 2x3) 10C 02-Aug-2003 08:58:12 LC/MS/MS #6 MRM of 4 Channels ES- 9.88 498 > 78 133583- 6.93e5 Area i G " ' '' , .... , .... 2.00 , .... , .... 4.00 , .... J .... 6.00 I .... _ .... 8.00 , " ...... 10.00 , .... ,Time 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103A, Ext.Date:08101/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Sun Aug 03 07:25=44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: S_tn Aug 03 07:32:25 2003 Page 39 Decatur BC BC 080103 Name: 080103A-2020 Text : i: C8 Acid L34910-10 (PFOA) 080103A-2020 Sm (Mn, 2x3) lqr0_ 02-Aug-2003 09:19:59_ LC/MS/MS #f_ MRM of 4 Channels ES- I 9.13 413 > 369I 195055- 1.13e6 Area ! t 0 I .... , .... I .... 2.00 , .... _ .... 4.00 %_ 2! C6 Sulfonate L34910-10 (PFHS) 080103A-2020 Sm (Mn, 2x3) , .... I .... 6.00 f .... J ....... 8.00 8.97 I'' "' I .... ,Time 10.00 12.00 02-Aug-2003 09:19:59 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 1i0-_ .... _ 'l ' [ I ' .... 2.00 _ ' IJ ' r _' ' Ill r ' , .... 4.00 _ .... 6.00 _ .... 108961 _I ' _'''"', .... _ .... 8.00 10.00 , .... i6T.7im1Aereae4 12.00 3:C8 Sulfonate L34910-I0 (PFOS) 080103A-2020 Sm (Mn, 2x3) ol0' .... , .... , ''"' 2.00 , .... J .... 4.00 W , .... ,"' 6.00 ' ' , .... 9.25 _' ," , , .... 8.00 02-Aug-2003 09:19:59 LC/MS/MS #6 MRM of 4 ChannelsES499 > 99 eA I .... 10.00 , .... i Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103A, Ext.Date:08101/03, Analys_K.Risha Sample List: Last modified_ Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103A Sun Aug 03 07z25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PR0\MethDB\Dacatur Sun Aug 03 07_ii:59 2003 Printed: S_n Aug 05 07:52:25 2003 Page 40 Decatur BC BC 080103 Name: 080103A-2020 Text : 4 : PFOSA L34910-10 080103A-2020Sm (Mn, 2x3) 02-Aug-2003 09:19:5_ LC/MS/MS#6 MRM of 4 ChannelsES- 9.91 498 > 78 Area 110-_ .... , .... _ .... ', , ,. , , .... 2.00 4.00 , .... , .... 6.00 133763_ , .... ,., '. , , .... u .... 8.00 10.00 6.89e5 _ .... ,Time 12.00 V Exy_en Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.=080103A, Ext.Date:08/01/03, Analyst:K.Risha SamPle List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PROkSam_leDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Maselynx\Fluoroch_micals.PRO\MethDB\Decatur Sun Aug 03 07=11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 41 Decatur BC BC 080103 Name: 080103A-2021 Text: i: C8 Acid (PFOA) L34910-10 Rep 080103A-2021Sm (Mn, 2x3) 1,,.__ 02-Aug-2003 09:41:47 LC/MS/MS #6 MRM of 4 ChannelsES- 9.13 167826- 413 > 369 9.66e51 Area; ! 0' .... , .... i .... 2.00 , .... , .... 4.00 %_ 2:C6 Sulfonate (PFHS) L34910-10 Rep 080103A-2021 Sm (Mn, 2x3) ii0 t '"' ' ' J .... , .... 2.00 J .... , .... 4.00 3:C8 Sulfonate L34910-10 Rep (PFOS) 080103A-2021Sm (Mn, 2x3) , .... , .... 6.00 * .... I .... 6.00 , .... ,. ,-,... 8.00 ,.,, .... 10.00 ,,,,. ,Time 12.00 02-Aug-2003 09:41:47 LC/MS/MS #6 MRM of 4 ChannelsES- 8.98 399 > 80 i_ .... , .... , .... ', .... 8.00 10.00 I "' ' ' ,Time 12.00 02-Aug-2003 09:41:4; LC/MS/MS #e MRM of 4 ChannelsES- 9.24 499 > 99 111 .... ,,,.., ,., ..., .... , .... 2.00 4.00 , .... , .... 6.00 , .... , ..1..0635_01.... , .... 8.00 10.00 ,, ... ,6T.i2m2eSArea 12.00 Ill Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:OB0103A, Ext.Date:08/01/03, Analyst=K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103A S_n Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslymx\Fluorochemicals_PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 42 Decatur BC BC 080103 Name: 080103A-2021 Text : 4 : PFOSA 534910-I0 Rep 080103A-2021 Sm (Mn, 2x3) ot 100_ 02-Aug-2003 09:41:47 LC/MS/MS #6 MRM of 4 ChannelsES- 9.90 498 > 78 191201- 9.92e5 Area ! .... , ,, , _ .... _ .... 4 , , ,', = , ,', ,' = .... , .... i .... , ....... 2.00 4.00 6.00 8.00 10.00 i .... _Time 12.00 V Ex1_en Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Maselynx\Fluorochemicals.PRO\Sam_leDB\080103A Sun Au_ 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 43 Decatur BC BC 080103 Name: 080103A-2022 Text : I: C8 Acid (PFOA) XC072503-3, 100 ng/L Standard 080103A-2022 Sm (Mn, 2x3) 02-Aug-2003 10:03:27 LC/MS/MS #6 MRM of 4 ChannelsES- 9.15 413 > 369 Area ! i 110_ 33920_ 2.02e5 _T-I , , , , i i _ ' J D , i , , , , _ , , , ,, , 1 , , , , , _ i , , ' , , , , , _, , , , '' i"; , , , _, , , ,,Time 2.00 4.00 6.00 8.00 10.00 12.00 %1,=/ 2:C6 Sulfonate (PFHS) XC072503-3, 100 ng/L Standard 080103A-2022 Sm (Mn, 2x3) 02-Aug-2003 10:03:2/ LC/MS/MS #6 MRM of 4 ChannelsES- 8.98 399 > 80 0 ' ' ' '-_'' ' ", .... 2.00 i ' ' '' , ' ' ' ' ,' L , , I ' ' ;-', 4.00 6.00 3:C8 Sulfonate (PFOS) iXC072503-3, 100 ng/L Standard 080103A-2022 Sm (Mn, 2x3) ' ' ' "-, " ' ' ' , ' "' ' , ' ' r, I-- ' ' * 1Time 8.00 10.00 12.00 02-Aug-2003 10:03:27 LC/MS/MS #6 MRM of 4 Channels ES- 9.25 499 > 99 .... ,,.,,, .... , .... , .... , .... , .... ,, ,', ,, .... ,.,-, ,-, ,., .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 V ExTgen Research, 3058 Research Drive, SLate College, PA 16801 %mlf Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Sample List : Last modified: Method: Last modified: Job Code : P: \Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\San_leDB\080103A Sun Aug 03 07:25:44 2003 P: \Data\LCMSMS6 \Masslynx\Fluorochemicals. PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 44 Decatur BC BC 080103 Name: 080103A-2022 Text : 4 : PFOSA XC072503-3, 100 ng/L Standard 080103A-2022Sm (Mn, 2x3) 1(0_ 02-Aug-2003 10:03:27 LC/MS/MS #6 MRM of 4 ChannelsES- 9.90 498 > 78 14698- 7.86e4 Area ! 0L'_,.., L .... _ .... 2.00 = .... _ .... 4.00 _ .... , .... 8.00 _ .... ,.'_ , , , ....... 8.00 10.00 i',-.. _Time 12.00 _l.,g Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 45 Decatur BC BC 080103 Name: 080103A-2023 Text : 1:C8 Acid (PFOA) XC072503-4, 250 ng/L Standard 080103A-2023 Sm (Mn, 2x3) 02-Aug-2003 10:25:1Q LC/MS/MS #6 MRM of 4 ChannelsES-i 9.13 413 > 369 Area ! 1_i/1 0' .... iJ:_',.., _. ,,' 2.00 I .... I .... 4.00 i .... , .... 6.00 79282_ .... _" ....... 8.00 I .... 10.00 4.72e5 _ .... _Time 12.00 _ 2:C6 Sulfonate (PFHS) IXC072503-4, 250 ng/L Standard 080103A-2023 Sm (Mn, 2x3) 14801 02-Aug-2003 10:25:1( LC/MS/MS #8 MRM of 4 ChannelsES- 9.02e4 Area _' ' ", ' "' ' , ' ' '" , .... t .... 2.00 4.00 : C8 Sulfonate (PFOS) XC072503-4, 250 ng/L Standard 080103A-2023 Sm (Mn, 2x3) _ .... , .... 6.00 , .... , .... 8.00 , .... , .... 10.00 , .... i Time 12.00 02-Aug-2003 10:25:1 LC/MS/MS #8 MRM of 4 ChannelsES- 9.25 499 > 99 100/I O'-,,,j V ,-.,, ,,,,. 2.00 j .... , .... 4.00 ,,,',, f,_,, 6.00 89651 _ .... , .... ', .... , .... 8.00 10.00 5.15e4Area i,,, ,,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Re_ort Set No.=080103A, Ext.Date:08/01/03, Analyst:K.Rieha Sample List: Last modified: Method: Last modified= Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Sun Aug 03 07=25:44 2003 P:\Data\LCMSMS6\Maeelyz_x\Fluorochemicals.PROkMethDBkDecatur Sun Aug 03 07=II=59 2003 Printed: Sun Aug 03 07:32=25 2003 Page 46 Decatur BC BC 080103 Name: 080103A-2023 Text : 4 : PFOSA XC072503-4, 250 ng/L Standard 080103A-2023Sm (Mn, 2x3) 1_=0_ 02-Aug-2003 10:25:1 LC/MS/MS #6 MRM of 4 ChannelsES- 9.92 498 > 78 34282- 1.79e5 Area 0 I.... ,.... _'' '" ,.... ,'''"'I"'''',' '"' ,.... i .... ,....... 2.00 4.00 6.00 8,00 10.00 i.... ,Time 12.00 V Fu_ygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:080103A, Ext.Date:08101103, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 47 Decatur BC BC 080103 Name: 080103A-2024 Text : i: C8 Acid L34910-11 (9FOA) 080103A-2024Sm (Mn, 2x3) 02-Aug-2003 10:47:0..= LC/MS/MS #3 MRM of 4 ChannelsES- 1 47341 2.88eE Area 11 ' i0_ , ,.. , .... , .... 2.00 , .... , .... 4.00 , .... , .... --_.. , . , ..9...126_1 .... _ .... 6.00 8.00 10.00 f-', , 4,1,3,T>im3e69i 12.00 %_ 2:C6 Sulfonace L34910-11 (PFHS) 080103A-2024 Sm (Mn, 2x3) 02-Aug-2003 10:47:05 LC/MS/MS #6 MRM of 4 ChannelsES- 8.96 399 > 80 O I_ I I ' I .... 3:C8 Sulfonate L34910-11 ' .... 2.00 (PFOS) _B ' ' I ' _ .... 4.00 080103A-2024 Sm (Mn, 2x3) 10 _ .... [ .... 6.00 I' .... I 8.00 ' ' I " I .... 10.00 12.00 ] ' 1 I' ' _ Time 235467 02-Aug-2003 10:47:0. _ LC/MS/MS #3 MRM of 4 ChannelsES- 1.27e7 Area /1 0"_ .... , .... _ .... 2.00 , .... , .... ., ....., .... 4.00 6.00 9.25 3_ , .... _ .... , .... , .... 8.00 10.00 499 > 9g , .... ,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:080103A, Ext.Date=08/01/03, AnalystzK.Risha Sample List: Last modified: Method: Last modified= Job Code: Pz\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11=59 2003 Printed= Sun Aug 03 07:32:25 2003 Page 48 Decatur BC BC 080103 Name: 080103A-2024 Text = 4 : PFOSA L34910-11 080103A-2024 Sm (Mn, 2x3) 1(_0_ 02-Aug-2003 10:47:05_ / LC/MS/MS #6I MRM of 4 ChannelsES- I 9.90 498 > 781 1215533- 6.18e6 Area 4 0 I .... _ . .',, , .... 2.00 _ ,'. , . J .... 4.00 r,,,, _ .... 6.00 , .... ,, ,.-, ,.,,, ..... 8.00 10.00 ,, ,, riTime 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set Mo.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 49 Decatur BC BC 080103 Name: 080103A-2025 Text: i: C8 Acid (PFOA) L34910-11 Rep 080103A-2025 Sm (Mn, 2x3) 02-Aug-2003 11:08:44 LC/MS/MS #6 MRM of4 ChannelsES- 9.12 413 > 369 Area 1 111 0 '1', . . , , .... , ,, ,", ,,, 2.00 '. , _ .... 4.00 ,,,_, 2:C6 Sulfonate L34910-11 Rep (PFHS) 080103A-2025 Sm (Mn, 2x3) 463017- L , .... ,, '. , . , .... ,'_ ...... 6.00 8.00 , .... 10.00 2.77e6 _ .... ,Time 12.00 02-Aug-2003 11:08:44 LC/MS/MS #6 MRM of 4 Channels ES- 8.96 399 > 80 Area 0i.., , .... , .... . _ . . ... , .... 2.00 4.00 : C8 Sulfonate L34910-11 Rep (PFOS) 080103A-2025 Sm (Mn, 2x3) , .... , .... 6.00 , .... , .... 8.00 _, ,.,. _ .... , .... ,Time 10.00 12.00 02-Aug-2003 11:08:44 LC/MS/MS #6 MRM of 4 ChannelsES- 9,26 499 > 99 11_ i1 .... J .... , .... ,.... ,,.,, 2.00 4.00 V .... , .... 6.00 1794353I. ,.... ,.... , .... , .... 8.00 10.00 1.00e7Ama ,.... ,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report q,_ Study No.:L34910, Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslymx\Fluorochem/cals.PR0\Sam_leDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 50 Decatur BC BC 080103 Name: 080103A-2025 Text : 4 : PFOSA L34910-11 Rep 080103A-2025 Sm (Mn, 2x3) 1,_,__ 02-Aug-2003 11:08:44 LC/MS/MS #6 MRM of 4 Channels ES- 9.87 929771- 498 > 78 4.73e6 Are_ I %=# ,, ,, .... , .... 2.00 , .... .j . .., . , .... , .... 4.00 6.00 ,,...,,, 8.00 r... , ....... 10.00 , .... ,Time 12.00 F_ygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _.,_ Study No.:L34910, Set No.=080103A, Ext.Date:08/01/03, Analyet:K.Risha Sample List: Last modified: Method: Last modified: Job Code: Pz\Data\LCMSMST\Massly_x\Fluorochemicals.PRO\Sam_leDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 51 Decatur BC BC 080103 Name: 080103A-2026 Text : i: C8 Acid (PFOA) L34910-20 080103A-2026Sm (Mn, 2x3) 100_ 9.12 404209- 02-Aug-2003 11:30:2g LC/MS/MS #6 MRM of 4 ChannelsES413 > 369 2.37e6 Area .... _ .... , ,,', ,, .... , .... 2.00 4.00 %mW 2:C6 Sulfonate L34910-20 (PFHS) 080103A-2026Sm (Mn, 2x3) , .... _, ,", ,, .... , .... 6.00 8.00 , , , , , .... 10.00 , .... ,Time 12.00 02-Aug-2003 11:30:2E LC/MS/MS #6 MRM of 4 ChannelsES- 8.96 399 > 80 1i0Y_l_' '' L .... _ .... 2.00 3:C8 Sulfonate L34910-20 (PFOS) _.. _, _ .... 4.00 060103A-2026 Sm (Mn, 2x3) , .... _ .... 6.00 _ .... , 2.3..3. 54_L'' 8.00 .. , .... 10.00 , .... ,1T.i4m1eAre_e_ 12.00 02-Aug-2003 11:30:2E LC/MS/MS #6 MRM of4 ChannelsES- 9.25 499 99 i111,0_ .... , .... , .... 2.00 r',.., , .... 4.00 ,... ,, .... 6.00 418516_ , .... , .... , .... _ .... 8.00 10.00 2.35e6Ares ,., .. ,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:080103A, Ext.Date:08101103, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103A Sun Aug 03 07725:44 2003 P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07732:25 2003 Page 52 Decatur BC BC 080103 Name: 080103A-2026 Text : 4 : PFOSA L34910-20 080103A-2026 Sm (Mn, 2x3) 1(IO-_ 02-Aug-2003 11:30:26 LC/MS/MS #6 MRM of 4 ChannelsES- 9.90 498 > 78 412369- 2.10e6 Area ! 0 l', , , , _ .... _,,,, 2.00 l, ,,, i .... 4.00 _,, ,', i .... 6.00 _ .... , r,,, 8.00 i", ...... 10.00 i .... i Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 _qp# Quantify Sample Study No.:L34910, ReDort Set No.:080103A, Ext.Date:08/01/03, Analyet:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 53 Decatur BC BC 080103 Name: 080103A-2027 Text : I: C8 Acid (PFOA) L34910-20 Rep 080103A-2027Sm (Mn, 2x3) 1(_ 02-Aug-2003 11:52:11 LC/MS/MS #6 MRM of 4 ChannelsES- 9.13 413 > 369 301201- 1.A76reea6 t 0 I .... ,.... , .... 2.00 _# : C6 Sulfonate L34910-20 Rep (9FHS) w"''', .... 4.00 080103A-2027 Sm (Mn, 2x3) , .... ,.... 6.00 ,.... , ....... 8.00 8.97 , .... 10.00 , .... ,Time 12.00 02-Aug-2003 11:52:11 LC/MS/MS #6 MRM of 4 ChannelsES399 > 80 1(o/1 0 t .... i .... _ .... 2.00 3:C8 Sulfonate L34910-20 Rep (PFOS) , .... J .... 4.00 080103A-2027 Sm (Mn, 2x3) 16649_ , .... _ ' ' Ti_' i .... I u'' ' ,, .... , .... 6.00 8.00 10.00 9.68e4Area , .... ,Time 12.00 02-Aug-2003 11:52:11 LC/MS/MS #6 MRM of 4 ChannelsES- 9.25 499 > 99 11i 0 J.... , .... , .... 2.00 , .... i .... 4.00 , .... i .... 6.00 2879331 , .... , .... , .... , .... 8.00 10.00 1.68e6Area , .... _Time t2.00 Exygen Research, 3058 Research Drive, Sta_e College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set NO.:080103A, Ext.Date:08101103, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A S_n Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\MethDB\Decatur S_n Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 54 Decatur BC BC 080103 Name: 080103A-2027 Text : 4: PFOSA L34910-20 Rep 080103A-2027 Sm (Mn, 2x3) 10C 02-Aug-2003 11:52:11 LC/MS/MS #6 MRM of 4 ChannelsES- 9.88 498 > 78 346884- 1.78e t Area C .... , .... r .... 2.00 , .... , . ,, 4.00 , , .... , .... 6.00 _'. ,-.. , .... 8.00 k , ....... 10.00 , .... ,Time 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %=j Study No.:L34910, Set No.:080103As Ext.Date:08101103, Sample List : Last modified: Method: Last modified: Job Code : P- \Data\LCMSMS6\Masslynx\Fluorochemlcals Sun Aug 03 07:25:44 2003 P : \Data\LCMSMS6 \Masslynx\Fluorochemicals. Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Analyst:K.Risha .PRO\Sam_IeDB\080103A PRO\MethDB\Decatur Page 55 Decatur BC BC 080103 Name: 080103A-2028 Text : i: C8 Acid (PFOA) L34910-21 080103A-2028 Sm (Mn, 2x3) 100_ 9.13 532619- 02-A ug-2003 12:13:52 LC/MS/MS #6 MRMof 4 ChannelsES413 > 369 3.15e6 Area 11 ' ''',' r""' ' t .... , .... , .... ' .... ' .... I .... , ....... 2.00 4.00 6.00 8.00 a .... 10.00 , .... i Time 12.00 _IF 2:C6 Sulfonate L34910-21 (PFHS) 080103A-2028 Sm (Mn, 2x3) 02-Aug-2003 12:13:52 LC/MS/MS#6 MRM of 4 ChannelsES- 8.98 399 > 80 1_0i/lI .... ., .... , .... 2.00 3:C8 Sulfonate L34910-21 (PFOS) _ .... , .... 4.00 080103A-2028 Sm (Mn, 2x3) , .... _ .... 6.00 , .... , 3..6..1721,...-. , .... 8.00 10.00 , .... ,2T.i1m1ee5Ares 12.00 02-Aug-2003 12:13:52 LC/MS/MS #6 MRM of 4 ChannelsES- 9.25 499 > 99 %e# 0" .... ,..... , .... 2.00 , .... ,.... 4.00 _ .... , .... 6.00 ,.... _ .... 8.00 , .... , .... 10.00 , .... ,Time 12.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, _ Set No.:080103A, Ext.Date:08/01/03, Analyst:K.Risha Sample List_ Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page B6 Decatur BC BC 080103 Name: Text: 080103A-2028 4: PFOSA L34910-21 080103A-2028 Sm (Mn, 2x3) 11_ 02-Aug-2003 12:13:52 MRM of4LCCh/MaSnn/MeSlsE#S6- 9.87 498 > 78 357273 Are_ ! 1.82e6 .... i .... , .... , .... J .... I .... i .... _ .... I .... c' ' ' b .... _..,. ,Time 2.00 4.00 6.00 8.00 10.00 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify San_la Study No.=L34910, Report Set No.:080103A, Fuct.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\San_leDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 57 Decatur BC BC 080103 Nama: 080103A-2029 Text : i: C8 Acid (PFOA) XC072503-5, 500 ngJL Standard 080103A-2029 Sm (Mn, 2x3) 100--_ 02-Aug-2003 12:35:3_ LC/MS/MS#6 MRM of 4 ChannelsES- 9.13 413 > 369 140009- 8.49e5 Are_ ] .... , '_"" *, .... _ ' , ' ' i .... 2.00 4.00 2:C6 Sulfonate (PFHS) XC072503-5, 500 ng/L Standard 080103A-2029 Sm (Mn, 2x3) 1 4 .... i .... 6.00 i '" ' ' , ....... 8.00 2849 L L .... 10.00 J .... i Time 12.00 02-Aug-2003 12:35:3_ LC/MS/MS #6 MRM of 4 ChannelsES- 1.72e5 Area i_ .... ', . '..., .... 2.00 , .... ; .... 4.00 3:C8 Sulfo_ate (PFOS) iXC072503-5, 500 ng/L Standard 080103A-2029 Sm (Mn,2x3) , .... , .... 6.00 , .... ; .8....98 1j .... , .... 8.00 10.00 _ .... 39,T9i>m8e0 12.00 02-Aug-2003 12:35:39_ LC/MS/MS #6_ MRM of 4 ChannelsES- I 9.24 499 > 99I 1to/1 171081 1.A02reea5 0_.., , _ .... , .... , .... , .... i .... J .... ",.. ,-. , .... , .... , .... i .... ,Time 2.00 4.00 6.00 8.00 10.00 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 | Quantify sample Report %_ Study No.:L34910, Set NO.=080103A, Ext.Date:08101103, Analyst=K.Risha Sample List: Last modified: Method: Last modified: Job Coda: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SazE_leDB\O8OlO3A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 58 Decatur BC BC 080103 Name: 080103A-2029 Text : 4 : PFOSA XC072503-5, 500 ng/L Standard 080103A-2029 Sm (Mn, 2x3) 1(O-_ 02-Aug-2003 12:35:39 LC/MS/MS #6 MFIM of 4 ChannelsES- 9.88 498 > 78 67231- 3.54e5 Area 0 .. ,",,, , . = .... 2.00 , .... , .... 4.00 ,.... _ .... 6.00 ,L , .... , ". , . ,, , , , .... 8.00 10.00 , .... ,Time 12.00 V Exyven Research, 3058 Research Drive, State Collage, PA 16801 Quantify Sa=_le Report _ Study No.:L34910, Set No.:080103A, Zxt.Date:08/01/03, _0_alyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslyllx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:ii:59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 59 Decatur BC BC 080103 Name: 080103A-2030 Text : i: C8 Acid (PFOA) XC072503-6, I000 n_L Standard 080103A-2030 Sm (Mn, 2x3) 02-Aug-2003 12:57:26 LC/MS/MS #6 MRM of 4 ChannelsES- 9.12 413 > 369 Area ! 11o/1 0 I .... , .',.., ,', , . , .... , .... 2.00 4.00 2:C6 Sulfonate (PFHS) X0072503-6, 1000 ng/h Standard 080103A-2030 Sm (Mn, 2x3) , .... ,.,,., 6.00 273386" _ .... i ....... ", .... 8.00 10.00 1.66e6 , .... ,Time 12.00 02-Aug-2003 12:57:26_ LC/MS/MS #6 I MRM of 4 Channels ES- t 8.98 399 > 80I 1to/1 0 I .... , .... , . . . , ,'. , , . ,'... 2.00 4.00 : C8 Sulfonate (PFOS) XC072503-6, 1000 ng/L Standard 080103A-2030 Sm (Mn, 2x3) ,','.... t .... 6.00 541981 i . ,-.. , .... , .... , .... 8.00 10.00 3.29e5Area , .... ,Time 12.00 02-Aug-2003 12:57:26 LC/MS/MS #6 MRM of 4 ChannelsES- 9.24 499 > 99 Area 0' .... J,",,, _ .... , .... _ ,,, ,, .... ,,,,, 2.00 4.00 6.00 i-. ,",, _ .... 8.00 _ .... , .... 10.00 , .... ,Time 12.00 Ex_gen Research, 3058 Research Drive, State College, PA 16801 Quantify san_le Report _ Study No.zL34910, Set No.:080103A, Ext.Date:08/01/03, Analyst=K.Risha Sample List: Last modified: Method: Last modified= Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\San_leDB\080103A Sun Aug 03 07:25:44 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07=Ii=59 2003 Printed: Sun Aug 03 07:32:25 2003 Page 60 Decatur BC BC 080103 Name: 080103A-2030 Text : : PFOSA XC072503-6, 1000 n_L Standard 080103A-2030 Sm (Mn, 2x3) 02-Aug-2003 12:57:2E LC/MS/MS #6 MRM of 4 ChannelsES- 129118- 6.85e5 Area 0'z',, . . , .... f .... 2.00 , .... , .... 4.00 , .... , .... 6.00 _ .... , .... 8.00 , ....... 10.00 _ .... ,Time 12.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 i Sl_or Study No P,xygea Study No: Analyte: loas Momtored: Site: NA 1,34910 PFOA 413 -> 369 Decatar Baker's Creek RAW DATA REPORT Limit of Qeanfitation: InjectionVolume: Malaix: Sample Weight: Final Volume'. 50 ppt 15 pL Soil 5.0 g 5.0 mL Set No." Analyst: InstnmaentType: Extraction Dam: Aaatyzed oa: 080103AR KareaRisha LCMSMS #6 08/01/03 08/04_3 Fx, ygen [13 XC072503-0 xc_2so_t xc072503.2 XC072503-3 xco_zso3.4 XC072503-5 XC077.503-6 Spomm ID Sxm_.<: Code CS cs Cs C__ cs CS CS Std. Ken Co_. No. _pt) 080103AR-301 0 0goio3_-3o2 zs 080103AR-303 50 080103AR-304 100 o8oto3_-305 2so 080103AR-306 500 080 t03Ag.307 1000 Diludoe Factor Peak Area 672 137t7 29040 51582 !13_98 242355 469994 Aaalyte Fcand (ppt) Amount Adtieti (ppt) peco_ery (%) Amdyte Foend fppb) Total Selid_ (%) Analytc Fo_mdLepb) D_ Wei_t 1.34910.1[ SpkE BC2 SED-06 LP 080L03AR-308 1000 3691 ** 5000 ] L34910-1 [ Spk E BCTS. ED-06 LF 080103AR-309 100 29373 ** 5000 ] L34910-20 Spk F Outfall to Rivet SED-25 LF 080103AR-310 100 28261 ** 5000 - ] i..34910-5 BC2 SED-04 S 080103AR-311 10 18223 ** 69.96 L34910-5 pep L34910-10 BC'2SED-04 BC2 SED-05 S 080103AR-312 S 080103AR-313 10 14512 ** 10 32594 ** 69.96 69.54 I 14910-10 Rep BC2 SED-05 S 080103AR-314 l0 31062 ** 69.54 XC072503-1 CS 080103AR-3 i5 25 12807 _'iBl_ XC072503-2 L34910-1 ! BC2 SED-06 CS 0g0103AR-316 50 25414 S 080103AR-3|7 1(30 9410 ** 60.41 L34910-I ! Pep L34910-1l I..34910-11 Rcp L349i0-20 L34910-20 Rep XC072503-3 XC0725034 L349 tO-7.0 BC2 SED-06 BC2S_ BC2 SED-06 Ouffall to River SED-23 Outfall to River SED-25 Outfalt to P,lve_ SED-2_ S 080[03AR-318 S 080t03AR-319 I00 9587 ** 10 80473 1780 S 080103AR-320 1O 76840 1700 S 080103AR-321 1(]4) 7081 ** S 080103AR-322 100 5379 ** CS 080103AR-323 i00 41160 CS 080103AR-324 250 96206 S O_t03AR-325 10 61092 t340 60.41 14.24 60.41 23.6 13.60 60.41 22.5 63.27 63.27 10.72 63.27 16.9 L34910-20 Rep L349tO-21 Outfall to River SED-25 Outfa/l to River SRD-25 Dup S 080103AR-326 S: 080103AR-327 10 44037 949 I00 I0169 * L349 i0-21 XC077,503-$ OetfaR to River SED-25 Dep S OgO103_Lg-328 C,$ 080103AR-329 500 i0 99240 22t0 215048 XC072503-6 CS 080i03AR-330 1000 406254 7.59 63.27 12.0 67.43 17.611 67.43 26.2 AnaJyteFotau(lppt) _ (peakarea- interceptI) slopex DF Recoverj (%) _ (aaal2"tte'ouad(ppt)-aJO_,tfeoum:iln control(ppt)l x i00 amoumadded(ppt) _ : Linear(l/x weighted) Inlercept= 2443.00 SIo_ = 438.457 Coef. Of Def. = 0.990236 Amdyte Found(ppb)= [a_Jyle found(ppt)x volumeextracted(0.04 L)] I sampleweight(5 8) Analyto Found (ppb)dry weight = analyle found (ppb)x (100% I tmal solids (%)) CS z Calibration standard C Coatrol sampI," S _ Sampte LF a Lab fofified samph_ FI: - Field fordfied sample LCS = LaboratoeyCono-o[Spike Cg _.Cheek Standard ND _, Not dctecugl. R_xaz_ between 0 and 25 ppt NQ = Not quantifiablea Reapoma: between25 ppt andLOQ (50 ppt) *Sample was analyzed with severai dilution factors in order to accommodate all compounds. The appropriate results arc reported. iii/i w $gensof StudyNo: Exygco.Study No:. Aaalyte: Iota Moral.toted: Site: NA L34910 PFOS 499 -> 99 DecaturBaker's Creek RAW DATA REPORT ' Limit of Quaaxitatiotu IJajtctiouVolume: Matrix: Simple Weight: FmaI Volume: 50 pt_t 15 pL Soil 5.0 g 5.0 mL Set No: AttaJ_tst: I_tmment Type: ExtractionDate: ,amalyzedon: 080103AR Ka.maRisba LCMSMS #6 08i01/03 08J04/03 Exygea ID XCD72503-0 XC072_03-1 XCOT25CO-2 XE072503-3 XC0"_7.503..4 XC077203-5 XC077203-6 I..34910-11 Spk E L34910-11 Spk E L349 t0.20 Spk F I..34910-5 L.34910-5 Rcp L34910-t0 L34910. tO Rep XC0'72503-1 XC072503-2 I..34910-11 L34910- I l Rep L3,1910-11 L34910- I 1 Pep L34910-20 L34910.20 Rep XC072503-3 XCO72503-4 L34910-20 I..34910-20 Rcp 124910-21 1,34910-2I XC072503d XC072503-6 Spoasm ID BC2 $I_D-06 BC2 SF.D-06 Omftli to River SED-25 BC2 SED-04 BC2 SEL)-04 BC2 SED-05 BC2 SED-05 BC2 SED-06 BC2 SED-06 BC2 SED-06 BC'2SED-06 OutfaJIto River SED-23 Oetfa]l to River SED*7.5 Outf=llto River SED-2.'| Ottffali to Pi,ver SED-2_ OuffaUto River SED-25 Dup Outfall to RiverSED-25 Dup Sample Code CS CS C..3 C.5 CS CS CS LF LF LF $ S S S CS CS S S $ S S S CS CS S $ S $ CS CS Run No. 080103AR-301 080103AR-302 080103AR-303 080103AR-304 080103AR.305 080103AR-306 080103AR-307 080103AR-308 080103AR-309 0BOtO3AR-3|O 0g0103AR-311 080103AR-312 080103AR-313 080103AR-314 080103AR-315 O_tOt03AP,-316 080103AR-317 080103AR-318 0BOIO3AR-319 080103AR-320 080103AR-321 080103AR-322 080103AR-323 080103AR-324 080103AR-325 080103AR-326 080103AR-327 O8OI03A.R-37.8 0g0 t03Ag-329 080103AR-330 Std. Cone. (ppt) 0 25 30 100 250 500 1000 25 50 100 250 500 I000 AnalyU.FOund(ppt)= (pe,ak area - intercept)/ slope x DF Recove.j7(%) = [analTtfound(ppc)-.analytfeouadin control(PP01x 1.00 am, otmtadded (ppt) Dilution Factor 10(30 10O t00 10 10 10 10 100 I00 10 10 100 100 10 10 100 IO Peak kP,,= 0 [442 3003 5613 I 1976 25896 51730 5387 51842 9506 9121 7449 14012 15401 1301 2860 66379 48518 526238 390663 6714 4609 4445 11649 65108 4_122 870t 80003 24473 44784 Analyte Found (pp0 Amount Added (ppt) Recovery (%) Analyte Formal (ppb) '_ 5000 ** 5000 19100 _ 1830 1490 2850 3130 ,,A _ ** ** 13400 9010 ** ** 17500 ** t 14 14.64 11.92 22.80 25.04 107.20 72.08 140.00 _ : Line_ (l/x weighted) ZaLr.rcep=t 254.789 Slo w = 48,3413 Coef. OfDet _ 0.991571 T_tl Solids (%) Aaalyt Found(9pb) . t:)t7WeiSht 69.96 20.9 69.96 17.0 69.54 32.g 69.54 36.0 60.41 60.41 60.41 60.41 63.27 169 63.27 114 63.27 63.27 67.43 208 67.43 AmulyteFouad (ppb) = {tnaiytefound (ppt) x v_Ltme extr_,'ted(0.04 L)] t sample weight ($ S) Amdyte Found (ppb)dry weight= a.nalytefound (ppb)x (100% / toUd solids (%)) CS _=C_ibzxtkm stamiatd C = Coatrol samp[e S = 5ample LF = Lab fortified ttmple 1_ = Field foetificd sample LCS = Labmatot3,ControlSpike CK = ChtmkStanda_ ND = Not det_t=d = Respommbetwetm0 mui25 ppt NQ _ Not quantifiable= Resfmmmbetween 25 pptandLOQ (50 ppt) Spreadsheetpreparedby:_/__3 **Sample was amdyz_ with several dilution factors in order to accommodate 811compounds. The apl_opriate results are reported. _[t_ AASampkm: quir_ reextrac_n. See data set 080603B. i i i SponsorStudyNo: ExygcnS_dy No: Analyte: Ions Mo_i*.oved: Site: NA L34910 FOSA 498 -> 78 Deca0n Bakes Creek RAW DATA REPORT Limit ofQuandtatlon: InjecdottVo|u_: Matrix: Samp_ Wei8t,,t: Final Volume: 50ppt 15 ytL Soil 5.0 Z 5.0 mL Set No: A.o._.lyst; In.strunTly_pte: ExCactionDate: Analyzed on: 080103AR K,ten R.isha LCMSMS #6 08/01/03 08104/03 _IIB_ Exygen to XC072503-0 XC072503-1 XC072503-2 XC072503-3 XC072503.-4 XC072503o5 XC072503--6 L34910-'t I Spk E L34910-I 1 Spk E L34910-20 Spk F L34910-5 L34910-5 Rep L34910-10 L34910-10 Kep XC072503-1 XC072503-2 L34910-11 L34910-'t I Rep I..34910-11 L34910-i I Rep 1.34910-20 1..34910-20 Rep XC072503-3 XC072503-4 L34910-20 L34910-20 Rep L34910-2L L34910-21 XC072503-5 XC072503-6 Sponsor _ BC2 SED-06 BC2 SED-06 Ouffall to I_iverSED-25 BC2 SED-04 BC2 SED-O4 BC2 SED-05 BC2 SED-05 BC2 SED-06 BC2 SED-06 BC2 SED-06 BC2 SED_6 Outfall to River SED-25 Ooffall to River SED-25 Ouffall to KiverSED-25 Ouffall to Riv_ SED-25 Outfall to River SED-25 Dup Outfall to River SED-25 Dup Sample coee CS CS CS CS CS CS CS LF LF LF S S S S CS CS S S S S S S CS CS S S S S CS CS Run No. 080103AR-301 080103AB.-302 080103AR-303 080 t03AB.-304 080103AR-305 080103AR-306 080103AR-307 080103AR-308 080103AR-309 080103AR-3 I0 080103AR-311 080103AR-312 080103AR-313 080103AR-314 080103AR-315 080103AR-316 080103AR-317 080103AR-3'18 080103AR-319 080103AR-320 080103AR-321 080103AR-322 080103AR-323 080103AR-324 080103AR-325 080103AR-326 080103AR-327 080103AR-328 080103AR-329 080303AR-330 Sad. Cone. Col+t) 0 25 50 100 250 500 1000 25 50 100 250 500 lO00 Dilution Factor t000 I00 100 I0 10 10 10 100 100 10 10 100 +t00 10 10 100 10 AJaalyteFound (ppl) = (peak area - inl_cept) / slope x DF Recovery (%) = [analy_efound (ppl)-ana]ytefound in control (ppt)]x 100 amount added (ppt) Peak ATe, 0 5040 10269 19684 45565 93155 179184 2308 21870 13524 16680 18189 19503 26862 4380 8991 21988 16805 200293 150384 6516 5371 17628 40103 61447 51717 9119 78207 86063 167421 Antly'te Found (ppt) Araount Added fro,6 Recovery ('/0) Analyte Found (ppb) ** 5000 '_ 5000 ** 5000 ** ** "* 1510 12.08 M _' ** ** *" ** 3500 2940 ** 4460 28.00 23.52 35.68 StandardCm'vc : Linear (l/x weighted) Intercept = 610.45 I Slope _ 174.067 Coef. Of Def. - 0.996985 To_.t Solids _O]o) - 69.96 69.96 69.54 69.54 60.41 60.41 60.41 60.41 63.27 63.27 63.27 63.27 67.43 67.43 AnalyteFound(ppb)= [analylefound(ppt)x volumeexlracted(0.04 L)J/ samplewc{ght(5 g) Analyl Found(ppb) dry weight = analyte found (ppb) x (10(Y'A/ total solids (%)) CS _ Cal_rsdon standard C = Controlsample S - Sample LF = Lab fortified sample FF = Fieldfortifiedsample LCS = LaboratoryControl Spike CK = Check Standard ND = Not detected_ Rcspo_sobetween0 and25 ppt NQ = Not quantifiable_ Response between 25 ppt andLOQ (50 ppt) **Sample was analyzed with several dilution factors in order to accommodate all compounds. _Sampie requires reextracdon. See data set 080603B. ,.+,.++++ The appropriate results arcreported. Analyte Found(ppb) Dr/Weip+ht . 17.4 44.3 37.2 52.9 ~ ks 5 cece B88000e 880088 sole. 2 g 2 | eo EERE RRRERR RR RRRRR RR NNT] 8 | $5 0092888888 1 ims ii 012800 1088 5 ll e i I 23 sp2eiiseseceliosssit "log3 corpsibgbzh oo. 5 I IEREEE: RR ARA EA C| 3h] ljtiimdiiecigagitisid : IF ie| 3Fo$h9b9b8s9a8a8aRE3a3i33i3i3s3h0e3s3a2n3a3i3a3s3i3i3n3s3s88s 53 SERRE RANA RRR RRRRARERARN] Bl Eni 15] pommmmma gs 3E3E3R3E53EEE 5E5E8R0EaEn0E00Rn8FEESHEH RERHRERGES $33: aasacessnissanenanenainnnnd -r i P 8i8 3 S939SE-amveonyQeoruoygILeney CNmeeenee2IERTREEERRANRIRSRERS 4) 0 0 _D LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA .Exygen Study No: L34910 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #6) Computer: Software: COMPAQ Professional Workstation AP200 Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Micromass Limited: MassLynx 3.4 Build 004 I-IPLCEquipment: Hewlett Packard (HP) Series 1100 I-IPBin Pump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column: Genesis C-8, 5 cmx 2.1 mm i.d. x 4 la (Exygen ID: 74A) (JONESCHROMATOGRAPHY: Part No. FK5962E) Mobile Phase (A) : 2 mM Ammonium Acetate in Type I Water /__ ! MAnoabliylest:Phase (B) : MKaertehnanRoilsha _)_/0_,/0"_ I Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 NOTE: The next 3 pages are computer generated printouts from the masslynx software program. The pages contain the instrument settings used for the analysis of this data set. All Handwritten Peak ID's by: _j_/o_/0'_ V Scanning Method Method: Last Modified: Report C:\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\C6 Thu Jul 31 16:23:50 2003 Page 1 C8 SULF C8 ACID PFOSA Printed: Mon Aug 04 07:47:13 2003 _I_I0 _ Solvent Delay ( mins ) : 0.00 Analog Channel Function :1 4 : Unused MRM of 4 Mass Pairs ( ESP- ) Inter Channel Delay ( Secs ) : Span ( Daltons ): Start Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 12.00 1 Dwell (Secs) Coll Energy (eV) Cone ( V ) 1 399.00 80.00 0.20 35 50 2 413.00 369.00 0.20 I0 I0 I 3 498.00 78.00 0.20 30 50 i 4 499.00 99.00 0.20 40 30 V Method Report Method File: Last Modified: C:\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\pfbs Monday, August 04, 2003 07_38;50 water Paga 1 _ Printed: Monday, August 04, 2003 07:47:18 _)l_1__ _ HPII00 LC Pump Initial Conditions Solvents A% B% C% D% 90.0 i0.0 0.0 0.0 Flow Stop Min Max Oven Oven (ml/min) Time (mins) Pressure (bar) Pressure (bar) Temperature Left(oC) Temperature Right(C) HPlI00 LC Pump Gradient Timetable 0.300 20.0 0 400 35.0 35.0 The gradient Timetable contains 8 entries which are : Time A% B% C% D% Flow Pressure 0.00 90 0 i0.0 0.0 0.0 0.300 400 i 2.00 90 0 i0.0 0.0 0.0 0.300 400 ! 5.00 i0 0 90.0 0.0 0.0 0.300 400 9.00 I0 0 90.0 0.0 0.0 0.300 400 9.50 00 100.0 0.0 0.0 0.300 400 14.00 00 i00_0 0.0 0.0 0.300 400 14.50 90 0 i0.0 0.0 0.0 0.300 400 20.00 90 0 I0.0 0.0 0.0 0.300 400 HPII00 LC Pump External Event Timetable The Timetable contains 6 entries which are : Time Initial 0.00 0.05 0.i0 11.90 12.00 Column Switch Off Off Off Off Off Off Contactl Off On Off Off Off Off Contact2 Off Off Off On Off off 'Contact3 Off Off Off Off On off Contact4 Off Off Off Off Off off HPII00 Autosampler Initial Draw Speed Eject Speed (#I/min) Draw Position (mm) Stop Time (mins) Injection Volume(_l) Vial Number Conditions 200.0 200 0.50 20.00 15.0 27 %.I Tuning Method: Method Report C : \MAS SLYIqX\ FLUOROCHEMI CALS. PROkACQUDB\FLUOROCHEMS Page 1 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Desolvation Temp. Temp. Pressures Analyser Gas Cell Vacuum Set 3.00 20 0.0 0.0 0.0 i00 300 Rdbk -2.93 -16 I00 299 Rdbk OFF 3.6e-3 AnalYser LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas Flows Cone Gas Desolvation V Set Rdbk 14.0 14.0 1.0 -2 ii " 15 21 2 14 14.0 14.0 2.0 650 -647 Rdbk 134.7 765.9 Quantify Calibration Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Calibration: Last modified: P:\Data\LCMSMS6\Masslynx\Fluoroche_icals.PRO\CurveDB\080103AR Tue Aug 05 07:30:00 2003 Printed: Tue Aug 05 07:31:58 2003 J__ Compound 1 name: C8 Acid (PFOA) Coefficient of Determination:0.990236 Calibration curve: 438.457 * x + 2443.00 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: l/x, Axis trans: None 4.70e5- Page 1 Decatur BC p_ u (____I_ _ x 4 Response- O: .... 0.0 , .... , .... 200.0 , .... _ .... 400.0 , .... , .... 600.0 , .... , .... 800.0 _ .... _ng/L 1000.0 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Calibration Report _ Study No.:L34910, Set No.:080103AR, Ext.Date:08101/03, Analyst=K.Risha Calibration: Last modified: Printed: P:\Data\LCMSMS6\Masslyn_\Fluorochemicals.PRO\CurveDB\080103AR Tue Aug 05 07:30=00 2003 Tue Aug 05 07:31:58 2003 Compound 2 name: C6 Sulfonate (PFHS) Coefficient of Determination:0.990051 Calibration curve: 77.0647 * x + 374.700 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: l/x, Axis trans: None 8.15e4- Page 2 Decatur BC x x 1 Response- V 0 .... 0.0 , .... , .... 200.0 i .... I .... 400.0 i'. ' ' ' , .... 600.0 , .... , .... 800.0 , .... ,ng/L 1000.0 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Calibration Report _mf Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Calibration: Last modified: Printed: P:\Data\LCMSMS6\Masslynx\FluorochemicalsPR0\CurveDB\080103AR Tue Aug 05 07:30:00 2003 Tue Aug 05 07:31:58 2003 Compound 3 name: C8 Sulfonate (PFOS) Coefficient of Determination:0.991571 Calibration curve: 48.3413 * x + 254.789 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: l/x, Axis trans: None 5.17e4- Page 3 Decatur BC x Response l,# 0 .... 0.0 , .... t .... 200.0 , .... _ .... 400.0 J .... , .... 600.0 , .... , .... 800.0 , .... ,ng/L 1000.0 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Calibration Report _ Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst_K.Risha Calibration: Last modified: Printed: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\080103AR Tue Aug 05 07:50:00 2003 Tue Aug 05 07731:58 2003 Compound4 name: PFOSA Coefficient of Determination:0.996985 Calibration curve: 174.067 * x + 610.451 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: l/x, Axis trans: None 1.79e5- Page 4 Decatur BC Response 0 .... 0.0 , .... , .... 200.0 , .... , .... 400.0 , ..... , .... 600.0 , .... , .... 800.0 , .... ,ng/L 1000.0 Exygen Research, 3058 Research Drive, State College, PA 168QI Q_antify Sample Re_ort Page 1 %_ Study No.:L34910, Set No.:0B0103AR, Ext.Date=08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code : Printed: P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\Sam_leDB\080103AR Tue Aug 05 07:24.:43 2003 P :\Data\LCMSMS6\Masslynx\Fluorochemicals. PRO\MethDB\Decatur Decatur BC BC 080103 Sun Aug 03 07:II:59 2003 _ _e Aug 05 07:32:01 2003 Indies Dale _l_Iol. u ' P_un#_blb_-_,,=T_o_ Name: 080103AR-301 Text : i: C8 Acid (PFOA) XC072503-0, 0 ngJL Standard 080103AR-301 Sm (Mn, 2x3) 110_ /_ _,',.. 2.00 _ .... , .... 4.00 _ .... _ .... 6.00 04-Aug-2003 08:35:50 LC/MS/MS #6 MRM of 4 ChannelsES- 4.35e4 Area 413 > 369_ 672 _ .... -_'_Time 8.00 10.00 V 2:C6 Sulfonate (9FHS) XC072503-0,0 ng/L Standard 04-Aug-200308:35:50 080103AR-301 Sm (Mn, 2x3) 0.90 1007 A 1.51 ' __ MRM of 4 ChannelsESLC/MS3IM99S > #8601 9_4 9.73 834 " . . . .,, , , ,, , ,, , _ .... , , , , , , .', ,, , , . , ,, . , , , , , , ,., .... _ .... 2.00 4.00 6.00 8.00 10.00 , ,, ,. Time : C8 Sulfonate (PFOS) XC072503-0, 0 ng/L Standard 060103AR-301 Sm (Mn, 2x3) 04-Aug-2003 08:35:56 LC/MS/MS #6 . MRM of 4 ChannelsES- 100_ 1.27 ,11 499 > 99 % 0_.9_ 012 _ .... I .... 2_'_'49.3 ...... ] .... 2.00 , .... , .... 4.00 s._3 _7 (' I' I I , .... 6.00 I .... 9 32 8.048.75 v_ "_- 9.92 , .... 8.00 , ..... , .... 10.00 1.96e.'. 11 4-_11.67 , .... Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample ReDort %_ Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103AR Tue Aug 05 07:24:43 2003 P:kDatakLCMSMS6\Masslynx\Fluorochemicals.PRO\MethDBkDecatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 2 Decatur BC BC 080103 Name: 080103AR-301 Text : 4 : PFOSA XC072503-0, 0 n_L Standard 080103AR-301 Sm (Mn, 2x3) 018 10 1 [ | 04-Aug-2003 08:35:50 LC/MS/MS #6 MRM of 4 ChannelsES- 998 1038 " " 498>78 2.00 4.00 6.00 8.00 10.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\Sam_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 3 Decatur BC BC 080103 Name: 080103AR-302 Text : i: C8 Acid (PFOA) XC072503-I, 25 n_L Standard 080103AR-302 Sm (Mn, 2x3) 1,,__ 04-Aug-2003 08:57:29 LC/MS/MS #6 9.13 13717- MRM of4 ChannelsES413 > 369 8.44e4 Area ! ! .... -..... ,_ , , _ .... -., ,_ 2.00 4.00 II_ 2:C6 Sulfonate (9FHS) XC072503-1, 25 ng/L Standard 080103AR-302 Sm (Mn, 2x3) 1,, _, ,,- ,,,,, 6.00 J , .... , . "-" 8.00 , --,-, ,_Time 10.00 04-Aug-2003 08:57:29 LC/MS/MS#6 MRM of 4 ChannelsES- 8.98 399 > 80 Area 0r-'_:_. ,---_;_,, , , , , , f _ , , , , , , , , , , , , , _ , , , , , , , , . , ,72,2.., 1_L .... 2.00 4.00 6.00 8.00 3:C8 Sulfonate (PFOS) XC072503-1, 25 ng/L Standard 080103AR-302 Sm (Mn, 2x3) 9.24 I ' ' ' "' i ' ' ' . 1T.4im2e4 10.00 04-Aug-2003 08:57:29 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 ,___ 2.00 4.00 6.00 8.00 10.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Area Quantify San_ple Study No.:L34910, Report Set No. :080103AR, Ext.Date:08/01/03, Analyst:K.Risha Ssm_le List: Last modified: Method: Last modified: Job Code : P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\Sam_leDB\O8OlO3AR Tue Aug 05 07:24:43 2003 P : \Data\LCMSMS6 \Masslynx\Fluorochemicals. PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 4 Decatur BC BC 080103 Name: 080103AR-302 Text : 4 : PFOSA XC072503-1, 25 ng/L Standard 080103AR-302 Sm (Mn, 2x3) 10C _ 04-Aug-2003 08:57:2. LC/MS/MS #E MRM of 4 ChannelsES- 9.92 498 > 78 5040- 2.63e4 Area C .... = .... 2.00_t'' ' _ .... 4.00.._.. i,,, ,6.0.0.._. _ .... 8.00..'.. _' ' '1'0.0'0'-' _'' ' ' Time i.i Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Rieha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluoroch_micals.PRO\Sa_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 5 Decatur BC BC 080103 Name: 080103AR-303 Text : i: C8 Acid (PFOA) XC072503-2, 50 n_L Standard 080103AFI-303Sm (Mn, 2x3) 04-Aug-2003 09:19:1 LC/MS/MS #1 MRM of 4 ChannelsES- 9.13 413 > 36g i1 1 Area t 4 C'-- ....... , .... 2.00 ,.... ,.... 4.00 _ .... _", , , , _ ,',,,, .-, , . , , , :.,".., . , .... 6.00 8.00 10.00 Time %_ 2:C6 Sulfonate (PFHS) XC072503-2, 50 ng/L Standard 080103AR-303 Sm (Mn, 2x3) 04-Aug-2003 09:19:12 LC/MS/MS #6 MRM of 4 ChannelsES- 8.96 399 > 80 03-_, , _ . , _ .... 2.00 , .... _ , , , , , . , , , , .... 4.00 6.00 3:C8 Sulfonate (PFOS) XC072503-2, 50 ng/L Standard 080103AR-303 Sm (Mn, 2x3) , , , ,,, , .... 8.00 , , ._-,-, .--_._. ,.: . ,n Time 10.00 04-Aug-2003 09:19:12 LC/MS/MS #6 MRM of 4 ChannelsES- 9.27 499 > 99 11_1% .......... I ' I - ' ' I-' ' -' ' I ' , ' ...l... ' ' l ' ' I ' ' 30: 0I3,_ , ' '-I ' _' '' ..... 2.00 4.00 8.00 8.00 10.00 1T.6im3e4Area Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07=11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 6 Decatur BC BC 080103 Name: 080103AR-303 Text : 4 : PFOSA FXC072503-2,50 n_L Standard 080103AR-303 Sm (Mn, 2x3) 04-Aug-2003 09:19:12 LC/MS/MS #6 MRM of 4 ChannelsES- 9.90 498 > 78 1(i/1 10269- [ 5.34e4Area 1 0 _'_,_ , , .... 4 .... , .... ', .... ,. ,.,,_ .... , .... , .... .,., ...... ,'.'.. , Time 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report %mJ Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha San_le List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\DatakLCMSMS6kMasslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07=32:01 2003 Page 7 Decatur BC BC 080103 Name: 080103AR-304 Text : !: C8 Acid (PFOA) XC072503-3, 100 ng/L Standard 080103AR-304 Sm (Mn, 2x3) 9.13 _ 04-Aug-2003 09:41:00( LC/MS/IVlS #6] MRM of 4 Channels ES- I 413 > 369 I 11o/1 51582 3.00e51Area It 0'_ ........ I .... I .... , .... I .... I .... _ .... I, _"' .... i,' '' I'' '"; Time 2.00 4.00 6.00 8.00 10.00 %_ 2:C6 Sulfonate (PFHS) XC072503-3, 100 ng/L Standard 04-Aug-2003 09:41:00 LC/MS/MS #6 080103AR-304 Sm (Mn, 2x3) MRM of4 ChannelsES- 8.96 399 > 80 1(07 IC' ;1, , . _,, , , , _ .... 2.00 8536' Y.... _ ' ' ' ' i .... _ '" ' ' , .... i ........J L 4.00 6.00 8.00 _" '" i .... 10.00 5.07e4 Arez Time 3:C8 Sulfonate (PFOS) XC072503-3, 100 ng/L Standard 080103AR-304 Sm (Mn, 2x3) 04-Aug-2003 09:41:00 LC/MS/MS #6 MRM of 4 ChannelsES- 9.25 499 > 9g 1(! 56131 3.18e4Are_ 0-', ,, ,--C_,,- ,, .... i .... , .... _ ,'_,,--, i .... _ .... i ;, , ,-r,', , , i , ,,,, ...,.. - Time V 2.00 4.00 6.00 8.00 10.00 Exy_en Research, 3058 Research Drive, State College, PA 16801 _qjf Quantify Sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103AR Tue Aug 05 07:24:43 2003 P=\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07=32:01 2003 Page 8 Decatur BC BC 080103 Name= 080103AR-304 Text - 4 : PFOSA XC072503-3, 100 ng/L Standard 080103AR-304 Sm (Mn, 2x3) 04-Aug-2003 09:41:00 LC/MS/MS #6 MRM of 4 ChannelsES- 9.92 498 > 78 lco/1 19684 1 1.0A3ree5a 1 0' .... _. ,. , , .... 2.00 , .... _,,., 4.00 ,,.., _ .... 6.00 , .... , , . '., .... i, ,',, _.... 8.00 10.00 Time V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sa_pleDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07=11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 9 Decatur BC BC 080103 Name: 080103AR-305 Text : i: C8 Acid (PFOA) XC072503-4, 250 ngJt Standard 080103AR-30SSm (Mn,2x3) 10 11379 04-Aug-2003 10:02:4(_ LC/MS/MS #6 I MRM of 4 Channels ES- I 6.66e5 Area 0 T ",,,, i_]/_w, ,"j .... 2.00 '1 F"' I ' I .... 4.00 2- C6 Sulfonate (PF_4S) XC072503-4, 250 ng/l Standard 080103AR-305 Sm (Mn,2x3) I .... J I, I"', ], 6.00 l II I I .... 8.00 10.00 Time I .... J I I_ I I r r ', , 04-Aug-2003 I0:02:4_ ClMS/M#S6I MRM of 4 Channels ES- f 8.98 399 > 80I 13' .... , .... _ .... 2.00 ,, ',', , , .... 4.00 3:C8 Sulfonate (PFOS) XC072503-4, 250 ng/L Standard 080103AR-305 Sm (Mn,2x3) _ ,".,. , .... 6.00 , .... , .... 8.00 _ .... _ , , ,', ,'. , . , Time 10.00 04-Aug-2003 10:02:40 LC/MS/MS #6! MRM of 4 ChannelsES- 9.25 499 > 9g IW __ .... _' ' '' .... 2.00 I .... I .... 4.00 I'I .... I ' '' ''I '' I; j_ ' ' Iq .... 6.00 8.00 { .... 10.00 -I ' '" ' Time Exygen Research, 3058 Research D_ive, State College, PA 16801 Quantify sa_le Report %_f Study No.:L34910, Set No.z080103AR, Ext.Date:08101103, Analyst:R.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochem/cals.PR0\Sam_leDB\080103AR Tue Aug 05 07x24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07zli:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page i0 Decatur BC BC 080103 Name: Text: 080103AR-305 4: PFOSA XC072503-4, 250 n_h Standard 080103AR-305 Sm (Mn,2x3) 04-Aug-2003 10:02:4C LC/MS/MS #6 MRM of 4 ChannelsES- 9.90 498 > 78 Ii/1 O' .... , .... ,...-'. 2.00 _ .... , .... 4.00 , .... , .... 6.00 , .... , .... 8.00 i , ....... 10.00 2A39reea5 , .... Time V V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:080103AR, Ext.Date:08101103, Analyst:K.Risha Sample List: Last modified: Method: Last modified:Sun Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\San_leDB\OSOlO3AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Massly_x\Fluorochemials.PRO\MethDB\Decatur Aug 03 07:11;59 2003 Printed: Tue Aug 05 07:32:01 2003 Page ii Decatur BC BC 080103 Name : 080103AR-306 Text : 1:C8 Acid (PFOA) [XC072503-5, 500 ng/L Standard !080103AR-306Sm (Mn, 2x3) 04-Aug-2003 10:24:2_ LC/MS/MS #6 MRM of 4 Channels ES- 9.14 413 > 369 1'1 242355- 1.40e6Are, 'l! 0"l .... ='_-_" ' , ' ' '"_ .... i .... , .... T.... _ .... _ ....... = .... ,, , ,_ Time 2.00 4.00 6.00 8.00 10.00 %_ 2:C6 Sulfonate (PFHS) XC072503-5, 500 ng/h Standard 080103AR-306 Sm (Mn, 2x3) 10 4332 04-Aug-2003 10:24:22 LC/MS/MS #6 MRM of 4 ChannelsES- 2.48e5 Area 0 I, , . i .... , .... 2.00 _ .... J'.'.-.. , .... , .... 4.00 6.00 3:C8 Sulfonate (PFOS) XC072503-5, 500 ng/L Standard 080103AR-306Sm (Mn, 2x3) _ .... _ .... i .... , .... , .... 8.00 10.00 Time 04-Aug-2003 10:24:22 LC/MS/MS #6 MRM of 4 ChannelsES- 9.27 499 > 99 1_l V 258961 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 1.A52rea5 Quantify Sample ReDort _ Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\Sam_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 12 Decatur BC BC 080103 Name: 080103AR-306 Text : 4 : PFOSA XC072503-5, 500 ngJL Standard 080103AR-306 Sm (Mn, 2x3) 04-Aug-2003 10:24:22 LC/MS/MS #6 MRM of 4 ChannelsES- 9.90 498 > 78 1_o/1 93155- tL 4.79e5Area 1 0", , , , .... , .... , .... _ .... , .... , .... , .... i .... , ....... , .... Time 2.00 4.00 6.00 8.00 10.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PROkSam_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMSS\Masslynx\Fluorochemicals.PR0\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: %h/e Aug 05 07:32:01 2003 Page 13 Decatur BC BC 080103 Name: 080103AR-307 Text: I: C8 Acid {PFOA) XC072503-6, 1000 ng/L Standard 080103AR-307 Sm (Mn, 2x3) 04-Aug-2003 10:46:0E LC/MS/MS #6 MRM of 4 Channels ES- 9.13 413 > 369 lql 0 I .... I'r" ' ' , .... . r .... , .... , ' ' ' ' _ .... 469994- L _ ,',""' , " ...... 2.69e6Area i .... J .... Time 2.00 4.00 6.00 8.00 10.00 _ 2:C6 Sulfonate (PFHS) XC072503-6, 1000 ng/L Standard 080103AR-307 Sm (Mn,2x3) 04-Aug-2003 10:46:0E LC/MS/MS #6 MRM of 4 ChannelsES- 8.96 399 > 80 0 l' '' ",' ",,, .... 2.00 _ .... _ .... 4.00 : C8 Sulfonate (gFOS) XC072503-6, 1000 ng/L Standard 080103AR-307 Sm (Mn, 2x3) , .... f .... 6.00 , .... _ .... , .... , .... _ .... 8.00 10.00 Time 04-Aug-2003 10:46:0E LC/MS/MS #E MRM of 4 Channels ES-: 9.25 499 > 99 Area .... ,.... _ .... , .... _ .... ,.... _ .... _ .... _ .... _ .... _ .... ,.... Time 2.00 4.00 6.00 8.00 10.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_IeDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 14 Decatur BC BC 080103 Name: Text: 080103AR-307 4: PFOSA XC072503-6, 1000 ng/i Standard !080103AR-307Sm (Mn, 2x3) 04-Aug-2003 10:46:08 LC/MS/MS #6 MRM of 4 ChannelsES- 9.91 498 > 78 Area I 1_1 0 j .... _ .... _ .... 2.00 ,' "' ' , .... 4.00 , .... i .... 6.00 , .... , .... 8.00 179184- , ....... 10.00 9.27e5 , ' '" ' Time W Exygen Research, 3058 Research Drive, State College, PA 16801 %=ef Quantify Sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha San_le List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemlcals. Tue Aug 05 07:24:43 2003 PRO\SampleDB\080103AR P:kDatakLC_SMS6kMasslynxkFluorochemicals.PROkMethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 15 Decatur BC BC 080103 Name: 080103AR-308 Text : i: C8 Acid (PFOA) L34910-11 Spk E, 5000 rig/L, DF=1000 080103AR-308 Sm (Mn, 2x3) 04-Aug-2003 11:07:51 LC/MSffvlS #6 MRM of 4 Channels ES- 9.13 413 > 369 1q0'/,,_,--:-_, A .,_,---_-T_,,.,, _,,,-.,, _T,I,I.I.,., ....3..6..9..1..-._... 2.44ea4 _ 2.00 4.00 6.00 8.00 10.00 2:C6 Sulfonate (PFHS) L34910-11 Spk E, 5000 ng/h, DF=1000 080103AR-308 Sm (Mn, 2x3) 100-_ 8.96 515_ I 04-Aug-2003 11:07:51 LC/MS/MS #6' MRM of4 ChannelsES399 > 80 3.50e3 Area 0 .... , . ,_'. f .... 2.00 , .... ,... 4.00 '.", .... , .... 6.00 3:C8 Sulfonate (PFOS) L34910-11 Spk E, 5000 ng/L, DF=1000 080103AR-308 Sm (Mn, 2x3) , .... _ .... _ .... r-.... , .... 8.00 10.00 Time 04-Aug-2003 11:07:51 LC/MS/MS #6 MRM of 4 ChannelsES- 9.25 499 > 99 , .. ..... _- , , , , ---,", , ,-- ' Time 2.00 4.00 6.00 8.00 10.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quaultify Sample Report %_ Study No.:L34910, Set No.:080103AR, Ext.Dats:08/01/03, Analyst:K.Risha San_le List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\SaE_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 16 Decatur BC BC 080103 Name: 080103AR-308 Text : 4 : PFOSA L34910-11 Spk E, 5000 ng/L, DF 1000 t080103AR-308 Sm (Mn,2x3) 04-Aug-20L0C3/MS1/1M:0S7:5#16 9.90 MRM of 4 Chann4e9l8s>ES78- t_2 ' 0 r' "-T'-T--T_I' .... I "' ' ' _ T _ . . - TT_. I .... I" ' ' ' I .... r .... I 2.00 4.00 6.00 8,00 10.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 17 Decatur BC BC 080105 Name: 080103AR-309 Text : i: C8 Acid (PFOA) L34910-11 Spk E, 5000 ng/L, DF=100 080103AR-309 Sm (Mn, 2x3) 1"" 04-Aug-2003 11:29:36 LC/MS/MS #6 MRM of 4 ChannelsES- 9.13 413 > 369 Area 1 .... _T>,,,. , .... 2.00 , .... ,, '.,, _ .... _ .... 4.00 6.00 , .... , ............... 8.00 10.00 1T.8im2ee5 %_ 2:C6 Sulfonate (PFHS) L34910-11 Spk E, 5000 ng/L, DF=100 04-Aug-2003 11:29:3E LC/MS/MS #6 080103AR-309 Sm (Mn, 2x3) 100 %. , , _ : i-, , , _'j-,_-, 2.00 , , , ,',', 4.00 , , i',, 6.00 MRM of 4 ChannelsES- 8.98 399 > 80 l46351 2.68e4 Area , __', , ,'=,_ .... 8.00 _ , , _ , _ , , _, _- , , , Time 10.00 3:C8 Sulfonate (PFOS) L34910-11 Spk E, 5000 ng/h, DF=100 080103AR-309 Sm (Mn, 2x3) o10',, , , ,.... , .... 2.00 , .... j .... 4.00 04-Aug-2003 11:29:3E LC/MS/MS #6 MRM of 4 ChannelsES- 9.25 499 > 99 1 _ .... _ ,, , , ,.... , ,', , ,.... _ .... _ .... 6.00 8.00 10.00 Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report I_ Study No.:L34910, Set No.:080103AR, _xt.Date:08/01/03, Analyst=K.Risha Sample List: Last modified: Method: Last m_dified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\DecaturBC Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 18 Decatur BC 080103 Name: 080103AR-309 Text : 4 : PFOSA L34910-11 Spk E, 5000 ng/L, DF=100 080103AR-309 Sm (Mn, 2x3) 04-Aug-2003 11:29:3E LC/MS/MS #6 MRM of 4 ChannelsES- 9.87 498 > 78 1_o/1 21870J- i 1.A12reea5 _t 0_, .-.. .... , .... _ .... , .... _ .... , .... , .... , .... ....... ,., , Time 2.00 4.00 6.00 8.00 0.00 _4 Exygen Research, 3058 Research Drive, State College, PA 16801 %_pr Quantify Sample Study No.:L34910, Report Set No.:0B0103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\O8OlO3AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur S_u_ Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 19 Decatur BC BC 080103 Name: 080103AR-310 Text : i: C8 Acid (PFOA) L34910-20 Spk F, 5000 ng/L, DF=100 080103AR-310 Sm (Mn, 2x3) 04-Aug-2003 11:51:14 LC/MS/MS #6 MRM of 4 Channels ES- 28261 1.66e5 Area ! 11/1 O_-_,, ,-'i--_, , , _ .... 2.00 _ .... _ .... 4.00 _ll# 2:c6 Sulfona'ce (PFHS) L34910-20 Spk F, 5000 ng/L, DF=100 080103AR-310 Sm (Mn, 2x3) ot 100_ , .... _ .... 6.00 9.1: _ k__ _ , _-,,_--_-_-_ ,. , , _ _, r-:i, 8.00 10.00 413 > 36g _, ,-Time 8.9d 4336- 04-Aug-2003 11:51:14 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 2.50e4 Area 2.00 4.00 3:C8 Sulfonate (PFOS) L34910-20 Spk F,5000 ng]L,DF=I00 080103AR-310 Sm (Mn, 2x3) 1CO-_ 6.00 8.00 10.00 9.2! 9506- 04-Aug-2003 11:51:14 LC/MS/MS #6 MRM of 4 Channels ES499 > 99 5.36e4 Area _W_J .... ,-, , ,T r" r _"'l .... _ , ,', , _ .... ,- , ,, ,',',, , _', .... 2.00 4.00 6.00 8.00 L , , ,, ,_"_,'_ .... 10.00 Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report _ Study No.iL34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Tue Aug 05 07:24:43 2003 Pi\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 20 Decatur BC BC 080103 Name: 080103AR-310 Text : 4 : PFOSA L34910-20 Spk F, 5000 ng/L, DF=100 080103AR-310 Sm (Mn, 2x3) 10h 04-Aug-2003 11:51:14 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498 > 78 13524- 6.94e4 Area j i .... T .... i .... i .... i .... i .... J .... _ ' '' ' 1 .... ", , ,".... _ ,;'. , , Time 2.00 4.00 6.00 8.00 10.00 V Furygen Research, 3058 Research Drive, State College, PA 16801 Quantify San_le Report %_ Study NO.:L34910, Set No.:080103AR, Ext.Data:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\Sam_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07::32:01 2003 Page 21 Decatur BC BC 080103 Name: 080103AR-311 Text : i: C8 Acid (PFOA] L34910-5, DF=10 080103AR-311 Sm (Mn, 2x3) 04-Aug-2003 12:12:52 LC/MS/MS #6 MP,M of 4 Channels ES- 9.12 413 > 369 Area I t 1i0_ '' '"T -T' ' ' i '_" "' I ' i-, , L , ''' 2.00 4.00 i .' ' ' , _ "_'_ 6.00 _ .... I ' 1:8r2_23L_ .... -_ ,-, , ' t .... ----"1T.0im6ee5 8.00 10.00 t_mJ 2:C6 Sulfonate (PFHS) L34910-5, DF=I 0 080103AR-311 Sm (Mn, 2x3) 04-Aug-2003 12:12:5,_ LC/MS/MS #6 MRM of 4 ChannelsES- 8.96 399 > 8(3 Area 1(i/0l .... r, , , , i .... , , 2.00 4.00 , .... , , 58.L, , .... , .... , .... 3T.7im3ee3 6.00 8.00 10.00 3:C8 Sulfonate (PFOS) L34910-5, DF=I 0 080103AR-311 Sm (Mn, 2x3) 100 A C ', , , , _ .... L',, , , _', ,', , t , 1-, , _ .... 2.00 4.00 04-Aug-2003 12:12:52 LC/MS/MS #6, MRM of 4 ChannelsES- 9.25 499 > 99 9121] 5.30e4 _--,,-, , _ , ,-.-, _ , , ,, 6.00 8.00 l Area ,, , ,Ti-, ' ' ' , _Time 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.=080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\San_pleDB\080103AR T_e Aug 05 07=24:43 2003 P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 22 Decatur BC BC 080103 Name: 080103AR-311 Text : 4 : PFOSA L34910-5, DF=10 080103AR-311 Sm (Mn, 2x3) 04-Aug-2003 12:12:5_ LC/MS/MS #6 MRM of 4 ChannelsES- 9.90 498 > 78 11 iyo .... I .... I .... I .... I .... I .... _ .... I .... i .... I 16..6..80 1 _,' ,_ .... 8.T6i7mee4Area .i 2.00 4,00 8,00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:kDatakLCMSMS6kMasslynx\Fluorochemicals.PROkSaz_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslymx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 23 Decatur BC BC 080103 Name: 080103AR-312 Text : i: C8 Acid (PFOA) [L34910-5 Rep, DF=10 080103AR-312 Sm (Mn, 2x3) 04-Aug-2003 12:34:39 LC/MS/MS #6 MRM of 4 Channels ES- 9.12 413 > 369 100o'/L1C-'_*.,_T_., , *'F', ' '-' i ' ''' _ .... _... ,-._.. ,,, 14,5,,1_ .... ", , . . , , ._Time8.59e4Area ' 2.00 4.00 6.00 8.00 10.00 2:C6 Sulfonate (PFHS) L34910-5 Rep, DF=10 080103AR-312 Sm (Mn, 2x3) 8.96 522"_ 04-Aug-2003 12:34:3S LC/MS/MS #6 MRM of 4 ChannelsES399 > 80 2.98e3 ........................ 2.00 3:C8 Sulfonate (PFOS) L34910-5 Rep, DF=10 080103AR-312 Sm (Mn, 2x3) 4.00 i .... _ .... , .... J .... _ .... L.... 6.00 8.00 10.00 Time 04-Aug-2003 12:34:39 LC/MS/MS #6 MRM of 4 Channels ES- 9.24 499 > 99 0- I ' I 'I' ' " f" I I r I } I I ' ' 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorocheunicals. PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 24 Decatur BC BC 080103 Name: 080103AR-312 Text : 4 : PFOSA L34910-5 Rep, DF=I0 080103AR-312 Sm (Mn, 2x3) 04-Aug-2003 12:34:3 LC/MS/MS #6 MRM of 4 ChannelsES- 9.87 498 > 78 110_ 181891 9.40e4Area i' .... _ .... _, ,., . , .... _ .... _ .... _ .... _ .... _ .... ,, ,-,, _,, ,.,% ,-_ , , Time 2.00 4.00 6.00 8.00 10.00 V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103AR Tue Aug 05 07=24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 25 Decatur BC BC 080103 Name: 080103AR-313 Text : i: C8 Acid (PFOA) L34910-10, DF=I 0 080103AR-313 Sm (Mn,2x3) 04-Aug-2003 12:56:21 LC/MS/MS #6 MRM of 4 ChannelsES- 9.12 413 > 369 O'-T, _ _ , t , "j , 2.00 2:C6 Sulfonate (PFHS) L34910-10, DF=10 080103AR-313 Sm (Mn, 2x3) ,,,, 4.00 0 '_' ' *" _ ' "' ' , .... 2.00 , .... I .... 4.00 3:C8 Sulfonate (PFOS) L34910-I0,DF=I 0 080103AR-313 Sm (Mn, 2x3) ,,,, ,, ,,, , 6.00 8.00 j , ,, , 10.00 , ,_ Time _ .... _ .... 6.00 04-Aug-2003 12:56:21 LC/MS/MS #6 ,64, 0 MRMof 4 ChannelsES- 8.96 399 > 80 0e, _ .... , .... 8.00 , .... , "' ' ' , .... 10.00 Area Time 04-Aug-2003 12:56:21 LC/MS/MS #6 MRM of 4 ChannelsES- 9.25 499 > 99 110] iI .... _ .... ,.... 2.00 _ , , , ,"f .... 4.00 140121 j . , , _ , , , ._ .... _ , ,', ,"j .... , .... 6.00 8.00 10.00 8.15e4Area _ .... ' Time Exygen Research, 3058 Research Drive, State College, PA 16801 %.4 Quantify Sample Study No.:L34910, Report Set NO.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\_luorochemicals.PRO\Sam_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MenhDB\Decatur S%zn Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 26 Decatur BC BC 080103 Name: 080103AR-313 Text : 4 : PFOSA L34910-10, DF=10 060103AR-313 Sm (Mn, 2x3) 04-Aug-2003 12:56:21 LC/MS/MS #6 MRM of 4 ChannelsES- 9.90 498 > 78 1(i/1 2.00 4.00 6.00 8'_.00 I 1950130_i.00 , .... 1T.0im1ee5Area ' 0 ' '" I _' _ "" '= ' $ I .... _ .... _ .... I .... l .... ['--' 'I .... .... .... V Exygen Research, 3058 Research Drive, S_ate College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:kData\LCMSMS6\Masslynx\Fluorochemicals.PRO\San_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 27 Decatur BC BC 080103 Name: 080103AR-314 Text : i: C8 Acid (PFOA) IL34910-10 Rep, DF=10 080103AR-314 Sm (Mn,2x3) 100_ 9.13 31062- 04-Aug-2003 13:18:10 LC/MS/MS #6 MRM of 4 ChannelsES413 > 369 1.85e5 Area 2.00 2:C6 Sulfonate (PFHS) L34910-I0 Rep, DF=I0 080103AR-314 Sm (Mn, 2x3) 4.00 6.00 8.00 8.96 10.00 04-Aug-2003 13:18:1G LC/MS/MS #6 MRM of 4 ChannelsES39o.>:380 110-_ ........ J .... 2.00 , .... , .... 4.00 3:C8 Sulfonate (PFOS) iL34910-10Rep, DF=I 0 080103AR-314 Sm (Mn, 2x3) ,' '"'' ]' ''' 6.00 1811_ i .... r .... _,, _ 8.00 10.00 1.10e4Area Time 04-Aug-2003 13:18:1G LC/MS/MS #6 MRM of 4 Channels ES- 9.25 499 > 99 101 0 t .... _ .... { ..I I ' '' 2.00 ' ' [ I ' _ .... 4.00 _ .... { .... 6.00 15401 1 9.18e4Area _ .... [ .... ' I i .' I t", J",' _ .... ' Time 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sam;le Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Ri_ha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochem/cals.PR0\SamDleDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PP4O\MethDB\Dacatur Su_ Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 28 Decatur BC BC 080103 Name: Text: 080103AR-314 4: PFOSA L34910-10 Rep, DF=10 080103AR-314 Sm (Mn, 2x3) 04-Aug-2003 13:18:1 LC/MS/MS #_ MRM of 4 Channels ES_ 9.87 498 > 72 Area 11_ 26862- 1.41e5 i "_''','' "' _ .... 2.00 , .... i .... 4.00 i .... t '"''',' 6,00 '"''', .... 8.00 , ' ' ' _ .... 0.00 T'' , . ' Time V , Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify sample Study No.:L34910, Report Bet No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 29 Decatur BC BC 080103 Name: 080103AR-315 Text : i: C8 Acid (PFOA) XC072503-I, 25 n_L Standard 080103AR-315 Sm (Mn, 2x3) 100-_ 9.13 12807- 04-Aug-2003 13:39:58 LC/MS/MS #6 MRM of 4 ChannelsES413 > 369 8.23e4 Area oL. ...... l 2.00 4.00 6.00 8.00 10.00 2:C6 %,# Sulfonate (PFHS) XC072503-1, 25 ng/L Standard 080103AR-315 Sm (Mn, 2x3) 04-Aug-2003 13:39:58 LC/MS/MS #6 MRM of 4 ChannelsES- 8.98 399 > 80 0 't--_'_-_-_' '_ -" '_ ' 'l , '"'' 2.00 _" " ' ' r .... 4.00 3:C8 Sulfonate (t_FOS) XC072503-1, 25 nglL Standard 080103AR-315 Sm (Mn, 2x3) I .... I .... 6.00 I I .... r ' -? "'_ .... _A t .... i" ," ,-," lime 8.00 10.00 04-Aug-2003 13:39:58 LC/MS/MS #6 MRM of 4 ChannelsES- 9.24 499 > 99 1'i/l 1301] 8.29e3 , , j .... , .... _ .... _ .... ,, .... ] .... _ .... ,-,,,, j,,,, _,,, , lime 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\DatakLCMSMS6kMasslynx\Fluorochemicals.PROkSamDleDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Stul Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 30 Decatur BC BC 080105 Name: Text: 080103AK-315 4: PFOSA XC072503-1, 25 ng/L Standard 080103AR-315 Sm (Mn, 2x3) il0 I .... , .... , .... _., , J .... 2.00 4.00 i .... , .... 6.00 , .... , .... 8.00 04-Aug-2003 13:39:58 LC/MS/MS #6 MRM of 4 ChannelsES- 9.89 498 > 78 Area , .... i .... 10.00 i, ,--_-_.Time V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last n%odified: Job Code: P:\Data\LCMSMS6\MasslyrLx\Fluorochemicals.PRO\Sam_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslyz_kFluorochemicals.PRO\MethDB\Decatu_ Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 31 Decatur BC BC 080103 Name: 080103AR-316 Text : i: C8 Acid (PFOA) XC072503-2, 50 ng/h Standard 080103AR-316 Sm (Mn, 2x3) 04-Aug-2003 14:01:43 LC/MS/MS #6 MRM of 4 ChannelsES- Area l __ i 0_-_, , ,_/_ ,_, _ .... I , , ,'_-_ .... _ .... _ .... i .._..L_ _ .... _ .... _ .... _ , _ 1T.5im0ee5 2.00 4.00 6.00 8.00 10.00 2:C6 Sulfonate (PFHS) XC072503-2, 50 ng/t Standard 080103AR-316 Sm (Mn, 2x3) 04-Aug-2003 14:01:43 LC/MS/MS #6 MRM of 4 ChannelsES- 8.96 399 > 80 0_- .......... _ ;, ,',' ,-,'.', _ ,', 2.00 4.00 3:C8 Sulfonate (PFOS) XC072503-2, 50 ng]L Standard 080103AR-316 Sm (Mn, 2x3) ,. r.'_ r,, ._-i .... ,_ ' 'r I''] , "1' ' ' , ' ' _-_' ' -- _ Time 6.00 8.00 10.00 04-Aug-2003 14:01:43 LC/MS/MS #6 MRM of 4 Channels ES- 9.25 499 > 99 1i_i__-T, , , "" ' ...I.. 2.00 V f ..... ' I 4.00 6.00 T r _ 1" T , , _ , ' " " _' ' ' l ' ' _ ' 8.00 ' ' ' ' _ ' " ' I '" ' ' ' 1T.6im6ee4Area 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/Gl/03, Analyst:K.Risha Sample List: Last modified: Method: Last m_dified: Job Code; P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\FlucrochemicalsPRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 32 Decatur BC BC 080_Q3 Name: 080103AR-316 Text : 4 : PFOSA IXC072503-2, 50 ng/L Standard 080103AR-316 Sm (Mn, 2x3/ 04-Aug-2003 14:01:43 LC/MS/MS #6 MRM of 4 ChannelsES- 1 8991 iI 2.00 4.00 6.00 8.00 10.00 4.83e4 Area %.# " V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/a3, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 33 Decatur BC BC 080103 Name: 080103AR-317 Text : i: C8 Acid (PFOA) !L34910-11,DF=I00 080103AR-317 Sm (Mn, 2x3) lr_r_ 9.11_ 9410 04-Aug-2003 14:23:27 LC/MS/MS #6 MRM of 4 Channels ES413 > 369 5.65e4 Area ,i L \ Time 2.00 4.00 6.00 8.00 10.00 2:C6 Sulfonate (PFHS) L34910-11, DF=100 080103AR-317 Sm (Mn, 2x3) 100_ 8.96 282-I 04-Aug-2003 14:23:27 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 2.13e3 %__ 0'-''-J.... ,., .,,, .... 2.00 3:C8 Sulfonate (PFOS) L34910-11, DF=100 ,.... -i ,, , , , .... .... 4.00 6.00 080103AR-317 Sm (Mn, 2x3) , .... ,.... 8.00 j .... '... , .... 10.00 Area Time 04-Aug-2003 14:23:27_ LC/MS/MS #6I MRM of 4 Channels ES- t 9.24 499 > 99I 0_ .... L .... _ .... _ .... _ .... _ .... t ' ' ' ' _ .... I .... _ .... ,,,,, _ .... Time 2.00 4.00 6.00 8.00 10.00 11_j, Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/03, A_lalyst:K.Risha Sample List: Last modified: Method: Last mmdified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 34 Decatur BC BC 080103 Name: 080103AR-317 Text : 4 : PFOSA L34910-II,DF=100 080103AR-317 Sm (Mn, 2x3) i10 j'l r ' ' J .... ' _ .... _ 2.00 _ I '" 4.00 [" I [ [ ' [' r ' 6.00 I I I '' I , .... 8.00 04-Aug-2003 14:23:27 LC/MS/MS #E MRM of 4 Channels ES- 9.89 498 > 78 i} .... , ' I ,',, .... 10.00 Oe Time V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last mmdified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Tue Aug 05 07:24:43 2003 P:kData\LCMSMS6\Masslynx\Fluorochemicals.PR0kMethDB\Decatur Su_ Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 35 Decatur BC BC 080103 Name: 080103AR-318 Text : i: C8 Acid (PFOA) L34910-11 Rep, D F=100 080103AR-318 Sm (Mn, 2x3) 9587 04-Aug-2003 14:45:17 LC/MS/MS #E MRM of 4 Channels ES- 5.66e4 Area_ 2.00 2:C6 Sulfonate (PFHS) L34910-11 Rep, DF=100 080103AR-318 Sm (Mn, 2x3) 100_ 4.00 6.00 ........ .... ................................. 2.00 4.00 3:C8 Sulfona_e (PFOS) L34910-11 Rep, DF=100 6.00 080103AR-318 Sm (Mn, 2x3) 1(0_ L__ , , ,,-"- Time 8.00 10.00 8.95 207-_ I 04-Aug-2003 14:45:17 LC/MS/MS #6 MRM of 4 ChannelsES399 > 80 1.56e3 Area .... Time 8.00 10.00 9.2.' 48518- 04-Aug-2003 14:45:17_ LC/MS/MS #6 I MRM of 4 Channels ES- I 499 > 99I 2.82e5 Area 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103/t_, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified= Method: Last modified= Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103AR Tue Aug 05 07:24=43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals. PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed= Tue Aug 05 07:32:01 2005 Page 36 Decatur BC BC 080103 Name: 080103AR-318 Text : 4 : PFOSA L34910-11 Rep, DF=100 080103AR-318 Sm (Mn, 2x3) 04-Aug-2003 14:45:17_ LC/MS/MS #6 I MRM of 4 Channels ES- I 9.89 _ 498 > 78I 1(i/l 168051 _ 8.6A3rea4 1' 0 L.... _ .... _ .... _ .... _ .... _ .... _ .... ._ .... _ .... _ ,. ..... ','_ .... Time 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify sample Study No.:L3&910, Repor_ Set No.:080103AR, Ext.Date:08/01/03, AnalystzK.Risha Sample List: Last modified: Method: Last modified: Job Code: P:kDatakLCMSMS6kMasslynxkFluorochemlcals.PROkSam_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Massly_x\_luorochemlcals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 37 Decatur BC BC 080103 Name: 080103AR-319 Text : i: C8 Acid L34910-11, (PFOA) DF=I 0 080103AR-319 Sm (Mn, 2x3) 1:,_, 9.11 80473- 04-Aug-2003 15:07:04 LC/MS/MS #6 MRM of 4 Channels ES413 > 369 4.67e5 Area i1 i .... 1', , , , _.... 2.00 _ .... _ .... 4.00 _ .... _ ,', ,, _ .... h ....... JL 6.00 8.00 i ' '' ' _', ''' 10.00 Time _ 2:C6 Sulfonate (PFHS) L34910-11, DF=10 080103AR-319 Sm (Mn, 2x3) 04-Aug-2003 15:07:04 LC/MS/MS #6 MRM of 4 Channels ES- Area 11!0 k i i ......1.............I i I 2.Q0 3:C8 Sulfonate (PFOS) L34910-11, DF=I 0 080103AR-319 Sm (Mn, 2x3) I 4.00 ]" I _I I r I I ' _ T--I ,_ 28I2-9' 5T5L, T ' I l I r r , I ' .. 3919T.3i>m68e04 6.00 8.00 10.00 04-Aug-2003 15:07:04 LC/MS/MS #6 MRM of 4 Channels ES- 9.25 499 > 99 11i=/o.... ,,, , ', _, ', ,", , .... ,, ',' ",' , _ .... _ .... 2.00 4.00 6.00 ,",, ',, [ 526238_ .... _ .... ='[ .... I .... 8.00 10.00 3T.0im5ee6Area _xygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Massly_c\Fluorochemicals.PRO\Sam_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslyrnc\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 38 Decatur BC BC 080103 Name: 080103AR-319 Text : 4 : PFOSA L34910-11, DF=I 0 080103AR-319 Sm (Mn, 2x3) 04-Aug-2003 15:07:04 LC/MS/MS #6 MRM of 4 ChannelsES- 9.87 498 > 78 O' .... , .... j .... 2.00 , .... i .... 4.00 , "' ' ' J .... 6.00 I .... i .... 8.00 i ....... 0.00 I"'' ,,'Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha SeaTtle List: Last modified: Method: Las_ modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: T_e Aug 05 07:32:01 2003 Page 39 Decatur BC BC 080103 Name: 080103A._-320 Text : i: C8 Acid (PFOA) L34910-11 Rep, DF=I 0 080103AR-320 Sm (Mn, 2x3) 1 i1.... L.... _.... 2.00 2:C6 %.# Sulfonate (PFHS) L34910-11 Rep, DF=10 , .... _ .... 4.00 080103AR-320 $m (Mn, 2x3) 04-Aug-2003 15:28:46 LC/MS/MS #6 MRM of 4 Channels ES- 7684 4.58e5 Area _ .... _, ,"' L .... , .... 6.00 8.00 i .... _ .... 10.00 _, ,'_, Time 04-Aug-2003 15:28:46 LC/MS/MS #6 MRM of 4 ChannelsES- 8.96 399 > 80 Area 0_,,,,, ,',,,,, ,", _ ,',',, _,, ,',, .... , .... 2.00 4.00 6.00 3:C8 Sulfonate (PFOS) L34910-11 Rep, DF=10 080103AR-320 Sm (Mn, 2x3) , .... , .... 8.00 , .... r', ,,, _ .... 10.00 Time 04-Aug-2003 15:28:46 LC/MS/MS #6 MRM of 4 ChannelsES- 9.25 499 > 99 " 110_ %,# 390663_ 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 2.30e6Area Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorocham/cals.PRO\Sam_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 40 Decatur BC BC 080103 Name: Text: 080103AR-320 4: PFOSA L34910-11 Rep, DF=10 080103AR-320 Sm (Mn, 2x3) 1 04-Aug-2003 15:28:46 LC/MS/MS #6 MRM of 4 Channels ES- 15038 7.59e5 Area ql,.#' .... , .... , .... , , , ,", , .... , .... J .... , .... ] .... j .... [ .... , .... 2.00 4.00 6.00 8.00 10.00 Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Re_ort Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last mmdified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\Sam_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 41 Decatur BC BC 080103 Name: 080103AR-321 Text : i: C8 Acid (PFOA) IL34910-20,DF=100 080103AR-321 Sm (Mn, 2x3) 1_ 9.12 7081- 04-Aug-2003 15:50:25 LC/MS/MS #6 MRM of 4 ChannelsES413 > 369 4.43e4 Area J 2.00 2:C6 Sulfonate (PFHS) L34910-20, DF=100 I080103AR-321Sm (Mn, 2x3) 100_ 4.00 .................... 6.00 8.00 10.00 ,,,, ,_ Time 8.98 334-_ I 04-Aug-2003 15:50:25 LC/MS/MS #6 MRM of 4 Channels ES399 > 80 2.23e3 Area ....... ' .......................................... 2.00 3:C8 Sulfonate (PFOS) L34910-20, DF=100 080103AR-321 Sm (Mn,2x3) 4.00 6.00 Time 8.00 10.00 04-Aug-2003 15:50:25 LC/MS/MS #6 MRM of 4 Channels ES- 9.26 499 > 99 11_0-- r ' ' ' [ .... , ,, 2.00 , ;' , .... J ' ' '_ _--' ' ' , '--' ' '--_.... "_''-'--6' 7'1_41.... T_-' ' _ _ ' '' 3T.9im6ee4Area 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\Sam_leD_\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 42 Decatur BC BC 080103 Name: 080103AR-321 Text : 4 : PFOSA L34910-20, DF=100 060103AR-321 Sm (Mn, 2x3) ot 100_ 04-Aug-2003 15:50:25 LC/MS/MS #6 MRM of 4 ChannelsES- 9.8E 498 > 78 6516- 3.40e4 Area _w_' .... i, 1 1_' , j ' T , I i--'] i , i '= }", i i, i_ '_=1 i _ ", ] i i _ .... j .... I .... _, .-m-, .... Time 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last mmdified: Method: Last mmdified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103AR Tue Aug 05 07:2_:43 2003 P:\Data\LCMSMS6kMasslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 43 Decatur BC _C 080105 Name: 080103AR-322 Text : i: C8 Acid (PFOA) L34910-20 Rep, DF=100 080103AR-322 Sm (Mn, 2x3) 10" 9.12 5379] 04-Aug-2003 16:12:07 LC/MS/MS #6 MRM of 4 ChannelsES413 > 369 3.44e4 O_, _ TAimreea i 2.00 4.00 6.00 8.00 10.00 %.J 2:C6 Sulfonate (PFHS) L34910-20 Rep, DF=100 080103AR-322 Sm (Mn, 2x3) 100-] 8.93 230] I 04-Aug-2003 16:12:07 LC/MS/MS #6 MRM of 4 ChannelsES399 > 80 1.76e3 Area ,-, .... - ........ 2.00 : C8 Sulfonate (PFOS) L34910-20 Rep, DF=100 080103AR-322 Sm (Mn, 2x3) -....... 4.00 ., ,., ., -................ 6.00 8.00 ,,, ..... 10.00 Time 04-Aug-2003 16:12:07 LC/MS/MS #6 MRM of 4 Channels ES- 9.24 499 > 99 %t.# 0 . , , ,1 ,, , , i- .... 2.00 j ,--,.,, , ,;',",-_-, 4.00 ,_, , ,_, , , ,', ;_, ,_ <, v .... , _ r, , , ,<,, 6.00 8.00 10.00 Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No:080103AR, Ext.Date:08/01/O3, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 44 Decatur BC BC 080103 Name: Text: 080103AR-322 4: PFOSA L34910-20 Rep, DF=100 080103AR-322 Sm (Mn, 2x3) 04-Aug-2003 16:12:07 LC/MS/MS #6 MRM of 4 Channels ES- 9.90 498> 78 1_1 53711 2.89e4Area i 2,00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, ReDort Set No.:080103AR, Ext.Date:08/Ol/03, Analyst:K.Risha San_le List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslymx\Fluorochemicals. PRO\Saur_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Page 45 Decatur BC BC 080103 Printed: Tue Aug 05 07:32:01 2003 Name: 080103AR-323 Text : i: C8 Acid (PFOA) XC072503-3, 100 ng/L Standard 080103AR-323 Sm (Mn, 2x3) # 04-Aug,2003 16:33:5C LC/MS/MS #6 MRM of 4 Channels ES- 41160 2.51e5 Area i .... _-, _ .... 2.00 _ .... . , _ _ . .... _ .... 4.00 6.00 2:C6 Sulfonate (PFHS) XC072503-3, 100 ng/L Standard 080103AR-323 Sm (Mn, 2x3) _ .... _ .... 8.00 _ , , ,T, , .... 10.00 , _ , , Time 04-Aug-2003 16:33:5 LC/MS/MS #6 MRM of 4 Channels ES- 8.98 399 > 80 0 _, , , _ .... , .... , .... , .'. ,. 1', , , ,', , , ,", _ .... T.... _ .... , .... _ .... 2.00 4.00 6.00 8.00 10.00 Time 3:C8 Sulfonate (PFOS) XC072503-3, 100 ng/L Standard 080103AR-323 Sm (Mn, 2x3) 04-Aug-2003 16:33:5 LC/MS/MS #6 MRM of 4 Channels ES- 9.24 499 > 99 11/1 0 t' ', ,'", ,l'_-_-', , , i', , r ' F "' ' ' / ' '"' ' I .... . , 4,4451 I ' ' [ '_ ' ' n' ' ' I .... I .... I .... 2.00 4.00 6.00 8.00 10.00 2.65e4!iArea Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha San_le List: Last modified: Method: Last modified: Job Code: P:\DatakLCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDBk080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 46 Decatur BC BC 080103 Name: 080103AR-323 Text : 4 : PFOSA XC072503-3, 100 ng/h Standard 080103AR-323 Sm (Mn, 2x3) 1 04-Aug-2003 16:33:5E LC/MS/MS #E MRM of 4 ChannelsES- 1762 9.31e4 Area i1 .... ._ .... L .... _ .... "L,"', r. _ .... _, ,',-, r'"... ,'_ .... L .... _ .... L .... 2.00 4.00 6.00 8.00 10.00 Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6kMasslyn_\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 47 Decatur BC BC 080103 Name: 080103AR-324 Text : I: C8 Acid (PFOA) !XC072503-4, 250 ng/L Standard 080103AR-324 Sm (Mn, 2x3) 100- 04-Aug-2003 16:55:35 LC/MS/MS #6 MRM of 4 Channels ES- 9.11 413 > 369 o/_ 1 i C .... _'-'_""' , .... I' ' ' ' I .... _ .... i ' ' ", _ .... i *, ,', I '' ' , I .... 1 .... 2.00 4.00 6.00 8.00 10.00 Time 2" C6 Sulfonate (PFHSI XC072503-4, 250 ng/L Standard 080103AR-324Sm (Mn, 2x3) 1 1704 04-Aug-2003 16:55:35 LC/MS/MS #6 MRM of 4 ChannelsES- 1.05e5 Area .................. 2.00 4.00 : C8 Sulfonate (PFOS} XC072503-4, 250 ng/L Standard 080103AR-324 Sm (Mn, 2x3) 6.00 ............ 8.00 10.00 Time 04-Aug-2003 16:55:35 LC/MS/MS #6 MRM of 4 ChannelsES- 9.24 499 > 99 1i0_ i],._ , c-, j I 2.00 ., . . , -_ _ 4.00 6.00 11649_ _ , .... -., , ,-, ,-j 8.00 10.00 6.79e4Are_ Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L54910, Set No.:080103AR, Ext.Date:08/01/05, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochem/cals.PRO\Sam_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: T_e Aug 05 07:32:01 2003 Page 48 Decatur BC BC 080103 Name: Text: 080103AR-324 4: PFOSA XC072503-4, 250 n_L Standard 080103AR-324Sm (Mn, 2x3) 04-Aug-2003 16:55:35 LC/MS/MS #6 MRM of 4 Channels ES- 9.89 498 > 78 1U/1 40103_ 2.14e5Area ' 0L,, , , _ .... _ .... _ .... _,,,, '_, ,,, l, ,,, _ .... { .... _ .... t .... f .... Time 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\Sam_leDB\080103AR Tue Aug 05 07:2&:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MetllDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:52:01 2003 Page 49 Decatur BC BC 080103 Name: 080103AR-325 Text : i: C8 Acid (PFOA) 534910-20,DF=I 0 080103AR-325 Sm (Mn, 2x3) 04-Aug-2003 17:17:20 LC/MS/MS #6 MRM of 4 Channels ES- 61092- 3.65e5 Area J 11_/1 9.11 413 > 369 i ot .... _' ' ' i .... 2.00 i r ' ' ' _ .... '_ .... ,.... 4.00 6.00 _ .... , ....... 8.00 , 4 "'"" _ i" ' ' ' Time 10.00 2:C6 Su!fonate (PFHS) L34910-20, DF=10 080103AR-325 Sm (Mn, 2x3) 04-Aug-2003 17:17:20 LC/MS/MS #6 MRM of 4 ChannelsES- 8.96 399 > 80 1i0_ 2.00 3:C8 Sulfonate (PFOS) IL34910-20, DF=10 080103AR-325 Sm (Mn, 2x3) 4.00 6.00 ,2:7_, L. ...._.... _ 8.00 10.00 1T.7im4e4Area 04-Aug-2003 17:17:20 LC/MS/MS #6 MRM of 4 ChannelsES- 9.24 499 > 99 '%,1, O r' ' ' ' I ' ' , ' i ' '" ' i .... i .... 2.00 4.00 I .... t .... 6.00 I .... _ .... 8.00 _ .... t .... 10.00 _ "' ' ' Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Re_ort Set NO.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\_CMSMS6\Massly31x\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 50 Decatur BC BC 080103 Name: 080103AR-325 Text : 4 : PFOSA IL34910-20, DF=I 0 080103AR-325 Sm (Mn, 2x3) 04-Aug-2003 17:17:20 LC/MS/MS #6, MRM of 4 Channels ES- 9.89 498 > 78 0 I .... , .... _ .... 2.00 _ .... r',', _, , .... _ .... 4.00 6.00 _,, ,',, .... 8.00 _ .... L.... 10.00 _ , , _', Time l..# Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6kMasslynx\Fluorochemicals.PROkMetllDBkDecatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 51 Decatur BC BC 080103 Name: 080103AR-326 Text : i: C8 Acid (PFOA) L34910-20 Rap, DF=I 0 080103AR-326 Sm (Mn, 2x3) 1 4403 04-Aug-2003 17:39:07 LC/MS/MS #6 MRM of 4 ChannelsES- 2.64e5 Area 0'_ ' ' ' , ...............,... , 2.00 %_ 2:C6 Sulfonate (PFHS) L34910-20 Rap, D F=10 080103AR-326 Sm (Mn, 2x3) , 4.00 j ' ....,... 6.00 , ' ' I-., ..... I ',, 'l' ' ", ' '" 'i . ' ,--_ Time 8.00 10.00 04-Aug-2003 17:39:07 LC/MS/MS #6 MRM of 4 ChannelsES- 8.96 399 > 80 1 0 P' ' ' ' _ ' "' ' ' _ .... 2.00 I .... _ .... 4.00 : C8 Sulfonate (PFOS) L34910-20 Rap, DF=10 080103AR-326 Sm (Mn, 2x3) I .... I .... 6.00 I ' '" ' '_ ' " ' ' _ .... I .... l .... ' |line 8,00 10.00 04-Aug-2003 17:39:07 LC/MS/MS #6 MRM of 4 Channels ES- 9.24 499 > 99 110 _ ii I .... _ .... _ .... 2.00 _ .... _ .... 4.00 , .... _ .... 6,00 451221 _,,,', _ .... _ .... _', ,,, _.... 8.00 10.00 2.6A3re8a5 Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6kMasslynx\Fluorochamicals.PRO\MethDB\Decatur Su_ Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 52 Decatur BC RC 080103 Name: 080103AR-326 Text : 4 : PFOSA L34910-20 Rep, DF=I 0 080103AR-326 Sm (Mn,2x3) 04-Aug-2003 17:39:07 LC/MS/MS #6 MRM of 4 Channels ES- 51717- 2.62e_ Arel 0 _.... t .... ,,,, 2.00 , , .... i .... 4.00 r .... i' '-_ ' J .... , .... 6.00 8.00 _ " ...... 0.00 i'' '" Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha San_le List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Massly_x\Fluorochemicals.PR0\MethDB\Decatur Su_ Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 53 Decatur BC BC 080103 Name: 080103AR-327 Text : i: C8 Acid (PFOA) L34910-21,DF=100 080103AR-327 Sm (Mn, 2x3) 04-Aug-2003 18:00:47 LC/MS/MS #6 MRM of 4 ChannelsES- 9.13 413 > 369 1(1_0 ...... -............... 2.00 2:C6 Su!fonate (PFHS) 534910-21, DF=100 080103AR-327 Sm (Mn, 2x3) 100_ ,', , _", , , , , 4.00 6.00 1016__L_ . ""6T.2im1ee4Area 'i 8.00 10.00 8.98 469] I 04-Aug-2003 18:00:47 LC/MS/MS #6 MRM of 4 ChannelsES399 > 80 3.35e3 Area , .............................. 2.00 3:C8 Sulfonate (PFOS) L34910-21, DF=100 080103AR-327 Sm (Mn, 2x3) 4.00 6.00 _ll,,=,J 2.00 0 ' I I I''"1 _ I ` I ' { .... 4.00 ' I ' _ [ _ " I ' %' { .... _ .... 6.00 , , ............ 8.00 10.00 , , ,,, "Time 04-Aug-2003 18:00:47 LC/MS/MS #6 MRM of 4 ChannelsES- 9.27 499 > 99 iioi ' I I ' _'l' ' 8.00 10.00 AeTime Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, ReDort Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:kDatakLCMSMS6kMasslynx\Fluorochemlcals.PRO\Sam_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tus Aug 05 07:32:01 2003 Page 54 Decatur BC BC 080103 Name: 080103AR-327 Text : 4 : PFOSA _L34910-21,DF=100 080103AR-327 Sm (Mn, 2x3) 04-Aug-2003 18:00:47 LC/MS/MS #6 MRM of 4 Channels ES- 9.89 498 > 78 1 J 0 ,_--_-_-,,_ ,,,, _, ,_-, _ ,-_, , ; ,. , j,,,, _ ,-,-, , , .... ,,,, ,, _-,, , ,._,, j,,, 1 Time 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha San_le List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochem/cals.PRO\SampleDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 55 Decatur BC BC 080103 Name: 080103AR-328 Text : i: C8 Acid L34910-21, (PFOA) DF=I 0 080103AR-328 Sm (Mn, 2x3) 04-Aug-2003 18:22:2_ LC/MS/MS #6 I MRM of 4 Channels ES- I 9.16 413 > 369] 0 L'' ''' , .... i .... ,''' 2.00 2:C6 Sulfonate (PFHS) L34910-21,DF=I0 080103AR-328 Sm (Mn,2x3) " , .... 4.00 _ .... , .... 6.00 i .... _ .... 8.00 ) .... i' "" ' _ .... 10.00 -rime 04-Aug-2003 18:22:2E LC/MS/MS #6 MRM of 4 ChannelsES- 8.99 399 > 80 1i0-_ ' ' '"'J'"'"-' ' , .... 2.00 3:C8 Sulfonate (PFOS) L34910-21, DF=I 0 , , .".. i .... 4.00 080103AR-328 Sm (Mn, 2x3) 5016_ _ , ,__ c;'. , ,-, ' , _. _ .... _ .... -j . . .- , ._-, 6.00 8.00 10.00 2.84e4Area Time 04-Aug-2003 18:22:2_ LC/MS/MS #6_I MRM of 4 ChannelsES- 9.28 499 > 99 iI. _.. ,, .... _ .... _ .... _,", ,'. _ .... _ .... _ .... _ .... L.... _ .... Time 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\San_leDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMS6\MasslynxkFluorochemicals.PR0\MethDBkDecatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 56 Decatur BC BC 080103 Name: 080103AR-328 Text : 4 : PFOSA L34910-21, DF=I 0 080103AR-328Sm (Mn,2x3) 04-Aug-2003 18:22:2_ LC/MS/MS #6 MRM of 4 Channels ES- 9.87 498 > 78 2.00 4.00 6.00 8.00 ""L 10{.00 _ .... Time .... I .... I'"' "'' '' .... I .... I .... I' r', r _ .... I r' I .... .... Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\080103AR Tue Aug 05 07:24:43 2003 P:\Data\LCMSMSS\Masslyr&_\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed= Tue Aug 05 07:32:01 2003 Page 57 Decatur BC BC 080103 Name: 080103AR-329 Text : i: C8 Acid (PFOA) XC072503-5, 500 ng/h Standard 080103AR-329 Sm (Mn, 2x3) :l0' .... , '--_' ' t .... 2.00 , .... _ .... 4.00 2:C6 Sulfona_e (PFHS) X0072503-5, 500 ng/h Standard 080103AR-329 Sm (Mn, 2x3) c'''' _ .... 6.00 04-Aug-2003 18:44:11 LC/MS/MS #6 MRM of 4 ChannelsES- 9.15 413 > 369 01 , .... , .... J .... J .... _.... 8.00 10.00 eea Time 04-Aug-2003 18:44:111 LC/MS/MS #E MRM of 4 ChannelsES- 8.99 399 > 801 1(i O t . , , _ .... J .,, 2.00 , .... J .... 4.00 3:C8 Sulfonate (PFOS) XC072503-5, 500 ng/h Standard 080103AR-329 Sm (Mn,2x3) 371831 2.23e51Areal J .... r." , , _ .... ,.... = .... ,.... J .... Time 6.00 8.00 10.00 04-Aug-2003 18:44:111 LC/MS/MS #6 MRM of 4 ChannelsES- 9.27 499 > 99 1i! .... %1,,I _ _,, ,, .... 2.00 _ .... ,-_. , _ .... _ .... 4.00 6.00 j ,,, , '_", ,2,,44731.... _ , ,' _', _ , _,, 1T.4imAere5eal 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\O8OlO3AR Tue Aug 05 07:124:43 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\Decatur Sun Aug 03 07:.11:59 2003 Printed: Tue Aug 05 07:32:01 2005 Page 58 Decatur BC BC 080103 Name: 080103AR-329 Text : 4 : PFOSA XC072503-5, 500 ng/L Standard 080103AR-329Sm (Mn, 2x3) 1 04-Aug-2003 18:44:11 LC/MS/MS #6 MRM of 4 ChannelsES- 86063 4.48e5 Area i Jk 0 I .... J .... _ .... , t'',' I .... , .... , .... t .... , .... h ....... _ .... Time 2.00 4.00 6.00 8.00 0.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No. :080103AR, Ext.Date:08/01/03, Analyst:K.Risha Sample List: Last modified: Method : Last modified: Job Code - P:\Data\LCMSMS5\Masslynx\Fluorochemicals.PRO\SampleDB\080103AR Tue Aug 05 07:124:_3 2003 P - \DatakLCMSMS5 \MasslynxkFluorochemicals. PROkMethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:32:01 2003 Page 59 Decatur BC BC 080 I03 Name: 080103AR-330 Text : I: C8 Acid (PFOA) XC072503-6, 1000 ng/L Standard 080103AR-330 Sm (Mn, 2x3) 04-Aug-2003 19:05:53 LC/MS/MS #6 MRM of 4 Channels ES- 9.15 413 > 36 11_ .... , .... r .,., 2.00 .... _ .... 4.00 2:C6 Sulfonate (PFHS) XC072503-6, 1000 ng/L Standard 080103AR-330 Sm (Mn,2x3) i1110_ .... ,.... ,.... 2.00 ,.... , .... 4.00 3:C8 Sulfonate (PFOS) XC072503-6, 1000 ng/h Standard 080103AR-330 Sm (Mn, 2x3) , .... r .... 6.00 ,.... _ .... 6.00 _ .... _ 4..0..6..2. 54- , J .... .... 2T.3im9eeEArea i, 8.00 10.00 04-Aug-2003 19:05:53 LC/MS/MS #6 MRM of 4 ChannelsES- 8.99 399 > 80 Area , .... ,7..1..5211_ .... ',,'. , , _. , . . 4T.1im9ee5 8.00 10.00 " 04-Aug-2003 19:05:53 LC/MS/MS #6 MRM of 4 Channels ES- 9.27 499 > 99 1ii,/o .... _h,#' , .... j .... 2.00 , .... , .... 4.00 _ .... _ .... 6.00 , ,, ,',, ....4478J4_,,, t ,'_ ,,, .... 8.00 10.00 2T.5im7ee5Area Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:080103AR, Ext.Date:08/01/03, Analyst:K.Risha San_le List: Last modified: Method: Last modified: Job Code : P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\San_leDB\080103AR Tue Aug 05 07:24:43 2003 P :\Data\LCMSMSI_ \Masslynx\Fluorochemicals. PRO\MethDB\Decatur Sun Aug 03 07:11:59 2003 Printed: Tue Aug 05 07:'32:01 2003 Page 60 Decatur BC BC 080103 Name: 080103AR-330 Text : 4 : PFOSA 'XC072503-6, 1000 ng/L Standard 080103AR-330 Sm (Mn, 2x3) 04-Aug-2003 19:05:53 LC/MS/MS #6 MRM of 4 Channels ES- 9.89 498 > 78 Area 1i_ _1_ _ 167421_ 2.00 4.00 6.00 8.00 10.00 8.67e5 %,,p' Exygen Research, 3058 Research Drive, State College, PA 16801 Sponsor Study No: Exygen Study No: Analyte: Ions Moedtored: Site: NA L34910 PFOS 499 -> 99 Decatur Bak=r's Creek RAW DATA REPORT Limit of Quantitation: Injet:tion Volume: Mat;fix: Sam pie Weight: "Final Volume: 50 ppt 15 _L Soil 5.0 g 5.'0 mL Set No: A.tmiyst: Instrument Type: Extraction Date: Analyzed on: 081203A Karen Risha LCMSMS #6 08/12,_3 08113/03 Exygpn Sponsor Std. A_alyte Amoum Analyte Total Anaiyte Sample Rua Cone. Dilution Peak Found Added l_:ovta 7 Found Solids Found (ppb) 113 xcogI103-O XC081 I03-1 I'D Code No. (ppt) Factm" Area (pp0 _pt) _%) (ppb) (%) Dr_ Weight CS 081203A-3001 0 0 CS 081203A-3002 25 909 XC081103-2 CS 0g1203A-3003 50 1896 XC081 f03-3 CS 08|203A-3004 100 3803 i XC081103-4 CS 051203A-3005 2.50 9700 ] XCOgl iO3-5 CS 0g 1203A-3006 500 19165 XC_,_81103-6 CS OrS1203&-3007 1000 39020 Methanol Wash C 0S 1203A-3008 0 Reagont Blank na C 0g I203A-3_19 0 ND Reagent Spk A Reagent Spk B na LCS 081203A-3010 na LCS 081203A-301 t 1963 49.2 50 98 21166 533 500 107 _$ttgl_ L34910-11 Spk E [..34910-11 Spk E XC081103-1 BC2 SED-06 BC2 SED-06 LF 051203A-3OI2 1000 8541 21.5000 100000 105 LF 0812CI3A.-3013 100 91234 1000OO CS 081203A.-3014 25 954 XC081103-2 XC08t 103-3 CS 081203A-3015 50 2208 CS 081203A-3016 100 4213 L34910-11 BC2 SED-06 S 081203A-3017 1000 4378 1104)00 880.00 60.41 1460 L34910-i I Pep 124910-11 BC"2 SED-06 BC'2 SED-06 S 081203A-301_, S 08t 203A-3019 -" 1000 100 4935 42296 124000 * 992.00 60.41 1640 60.41 I..34910-11 Pep XC081 I03-4 XC0g1103-5 XC081103-6 BC2 SEDd}6 S 081203A.3020 1{]0 48356 * C.S 081203A-3021 250 11039 CS 081203A-3022 500 20668 CS 081203A-3023 I000 39291 60.41 Analyte Pound (Pp0 = (peak area - intemep0 / slope x DF Rccovcxy (%) = [am_yte fomad (ppt_te found in condor (ppt)] x tOO . amount addcct (ppt) _ : Linear (l/x weigh,_d) httet_ept _ 10.4732 Slope = 39727 Conf. Of Dot. = 0.998540 $_nalyte Found (ppb) = [ana]yte fotzud (PP0 x vohtme xUacw.,d (0.04 L)] / sample weighL (5 g) Analyte Found (ppb) dr,/weight = analytefouad (ppb) x {10(_e / total anlid* (%)) CS = Calibration standard C = Conuol sample S a, Sample LF = Lab fortified sample FF = Field fortified sample LCS = Lal3oratory Control Spike CK w Ch_k Standard ND = Not detected = Response betweea 0 and 25 ppt NQ - Not quantifiable m Response between 25 ppl and LOQ (50 ppt) Dilutionwas for PFOSA. V II #_11 Sponsor Study No: Exygen Study No: Analyle: Ions Monitored: Site: NA L34910 FOSA 498 -> 78 Decatur Baker's Creek RAW DATA REPORT Limit of Quantitation: lnj gttion Volume: Marx: Sample Weight: Final Volume: 50 ppt 15 _L Soi', 5.0 g 5.0 mL Set No: Analyst: Ins_xument Type: Extraction Date: Analyzed on: 081203A Kar_ Risha LCMSMS _6 08/12/03 0g/I 3/03 Exygen I13 XC081103-0 XC081103-1 XC081103-2 XC081103-3 XC081103-4 XC081103-5 XC0$1 |03-6 MeOaa.noi Wa_ Reagent Bhmk Reagent Spk A Reagent Spk B L349lO-11 SpkE L34910-11 SpkE XC081103-1 XC081 t03-2 xc0gII03-3 L34910-11 L34910- I I Rep L3491 O- ! I L34910-11 Rcp XCO81103.-4 XCOg1103-5 XC081103-6 Sponsor ID i_a na na BC2 SED-06 BC2 SED-06 BC2 SED-06 BC2 SED-06 BC2 S ED-06 BC2 SED-06 Sample Code CS CS CS CS CS CS CS C C LCS LCS LF LF CS CS CS S S S S CS CS CS Rua No. 081203A-3001 081203A-3002 081203A-3003 081203A-3004 081203A-3005 081203A-3006 0812(13A-3007 051203A-3008 Og 1203A-3009 081203A-3010 081203A-30] 1 081203A.3012 081203A.3013 0g 1203A-3014 081203A-3015 0g1203A-3016 081203A-3017 081203 A-3018 081203 A-3019 081203A-3020 081253A-3021 Og t203A-3022 081203A-3023 Aaalyt Found _pt) Recovery (%) = _ (p_ak _ea - intc_cep0 / slope x DF [anal),m found (ppt)-anal_te found in con_'ol m_otmt added (PPO (ppt)] x I00 Std. Cone. (_pt), 0 25 50 IOO 250 500 I000 Dilution Factor 25 50 100 250 500 IOOO I000 100 I000 10OO 100 100 Peak Arei 0 3547 7692 15522 39080 73905 145023 0 0 7255 72614 11415 122331 4230 8197 16248 14.46 1737 13834 16015 41122 78848 149443 Analy'tc Found (ppt} Amotmt Added (plat) Recovery (%) Analyle Found (_lah) ND 45.5 50 91 481 500 96 " 100000 812_, |OGO00 72 * * 8930 10400 71.44 83.20 Standar,_l _q.rv : Linear (l/x tntcrcepI - 434.45J Slope = 150.037 Coet_ OlDer. = 0.998129 weighted) Total So'rids /*A) 60,41 60.4 I 60.41 60.41 Analytc Found (pph) = [analyte found (ppt) x volume extracted (0.04 L)] / sample weight (5 g) Ana|_e Found (ppb) dry weight = _maly_e found (pph) x (100% / total solids (%)) CS = Cal_rafioa standard C " Control sample S = Sample LF _ l_h fortified sample FF _ Field fortified sample LCS = Laboratory Con_ro| Spike CK = Check Standard ND _ Not detected _ Response between 0 and 25 ppt NQ = Not qttantifiable = Kespunse between 25 lapt and LOQ (50 PP0 Analyte Found (ppb) D_ Weight I 18 138 Dilution was for PFOS i: " TM! P,E S E A R C H State College, PA 16801 Fax: 814-231-1580 SAMPLE TRANSFER SHEET Protocol Number: Exygen Sample # L34910-11 NA Sponsor Sample # BC2 SED-06 Exygen Study Number: Exygen Sample # L349 I0 Sponsor Sample # Karen Risha 08/11/03 1400 Requested By (Printed Name/Date/Time) Samples removed from: ._:g:t_ -f"lP'_, Samples removed from: _ Box# _ Box# _ Shelf# _. Shelf# Samples transferred to the custody of _P_ A_:_,*'f_ [e_ g-//-sz /P'_o Sample Custodian Initials/Date/Time Samples received from custodian; Samples moved to /_e - 30_ Laboratory Personnel Initials/Date/Time ql_ Samples returned to _'_,"/'9_"_ 9 .. _ _,_/_...,_5 ,_.._0 Sample Custodian Initials/Date/Time Egen .H State College, PA 16801 Fax: 814-231-1580 _,,I Internal Chain of Custody/Fortification Sheet Exygen Study Number: L34910 Matrix: Soi___jl Sponsor Study/Protocol No: NA The samples listed below were removed from refrigerator No. Time d_[_" CLIENT SAMPLE ID ...... Date t_/l_/t9__ EXYGEN ID NUMBER WEIGHT (g) Initials FORTIFICATION (rig) na Reagent Blank na .. Reagent Spk A 2,0 na Re.a.[entSpk B 20.0 BC2 SED-06 L349t0-11 Spk E 5.0 4000.0 BC2 SED-06 L34910-11 5.0 BC2 SED-06 L34910-11 R.ep 5.0 1.,I - _ Reagent Spk A Rea_entSpkB L34910-11 Spk E Spiking Solution Used F061103-2 (I0 n__/m.L) F061103-1 (100ng/mL) F060203-1 (I0000 n_mL) m, - m, Volume Used for Spiking .200 laL (200 I.tLmicropipet) . [.nitial/Date _" [t_12.,lO" 200_L(20Ok_LmJcropipet ) _ 400 _L (200 _tL micropipet) . _'- U /_,IJZlO:. /b_ 112_0 All samples were weighed on balance No. _)., t_m_ _q_ Da_ea_//Z/O__ -I 1 Ini_als_ After weighing samples were returned to re/fn'_erator No. _. Comments: / t. 2o0 !aLof 250 mg/mL sodium thiosulfate was added to all samples before spiking. Initials/Date: _.____ Analysis Summary: Data Set: _t2.0_A Data Set: -- Data Set" _ Initials/Date: ___._llla'-i"-o_)113162'_ Initials/Date: _. _- Initials/Date: _ /- Set extraction/analysis data verified by_f Date: _//_Ju'/4ly_ 26, 200111 a; . EA 33it i0 Hod| |La EBFEHiHl t TmlT:oeI|]| | ~i 5 it H2oig2, HET SFhH oH] di: HH || SELH Hii ; y 1] Hine TI li | :H ll ~~ ) if f ! } ji Li i SS| EEgees III mmll I ww |B] so | 1 e & 2 Bs BES 1 niin 3 | gF6R li I3E J 2 EI, BB | & Bed i | Fala eseaRRiTEEN ! | | oriiriniiiiinitian C|Bi| HghaamaaHlI a2,8 g2i25d | E 81 R 35E a, tA heater Han . 1 Humiiibims || EkBZ 2Sinn [8 i $3 p|, q55 5& w|i 8 f a in EEE BEEEEERTEZcscEicessssit 23333333233333333333333 E racrnongIuenRrfaoonn 12 i | FanTnenea2INRIRLERRRANR CD 00_ ! r 13. o E > a o _ EEEEEEEEEE EEEEEEEEEEEEE o ._ _ _m X_ _9 __ m_ ___ 00000000000000000000000 = QQQQQQQQo_o_eeooooooooo <<<<<<<<<<<<<<<<<<<<<<< = SS DDDD SDD :====o=S_=oo=oS oooooooooooooooooooo_oo LC/MSIqVIS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exygen St.ud, y No: L34910 Instrument: Micrornass Quattro Ultima (LC/MS/MS Unit #6) Computer: Software: COMPAQ Professional Workstation AP200 Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Micromass Limited: MassLyn.x 3,4 Build 004 HPLC Equipment: Hewlett Packard (t-IP)Series 1100 HP Bin Pump I-IPVacuum Degasser lip Autosampler I-{PColumn Oven I-IPLCColumn: Genesis C-8, 5 cmx 2.1 mm i.d. x 4 p (Exygen ID: 74A) (JONESCHROMATOGRAPHY: Part No. FK5962E) Mobile Phase (A) : 2 mM Ammonium Acetate in Type I Water a_ Mobile Phase (B) : Methanol ,1 _ N_\O__'_ 1 Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 ]?hone: (814) 272-i039 FAX: (814) 231-1580 NOTE: The next 3 pages are computer generated printouts from the masslynx software program, The pages contain the instrument settings used for the analysis of this data set. All Handwritten Peak ID's by: _D_ I_! 0_ Scanning Method Report q_ Method: C:\MASSLYNX\}_UOROCHEMICJLLS.PRO\ACQUDB\C6 Last Modified: Thu Jul 31 16:23:50 2003 C8 SULF C8 ACID PFOSA Page 1 Printed: Solvent Delay Wed Aug 13 09:37:33 2003 ( mins ) : 0.00 _511_I_ _ Analog Channel Function :1 4 : Unused MRM of 4 Maa:s Pairs ( ESP- ) Inter Channel Delay (Secs ): Span ( Daltons ): Start Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 12.00 1 Dwell (Secs) Coll Energy (eV) Cone ( V ) 1 399.00 80.00 0.20 35 50 2 413.00 369.00 0.20 i0 I0 i 3 498.00 78.00 0.20 30 50 4 499.00 99.00 0.20 40 30 Method Report Method File: Last Modified: C:\MASSLYNX\FLUOROCHEMICALS.PRO\ACQUDB\pfbs Wednesday, August 13, 2003 09:25:46 m, water Page ! HPII00 LC Pump Initial Solvents A% B% C% D% Conditions 90.0 i0.0 0.0 0.0 Flow Stop Min Max Oven Oven (ml/min) Time (mins) Pressure (bar) Pressure (bar) Temperature Left(C) Temperature Right(C) 0.300 20.0 0 400 35.0 35.0 HPII00 LC Pump Gradient Timetable The gradient Timetable contains 8 entries which are : Time A% B% C% D% Flow Pressure 0.00 90.0 i0.0 0.0 0.0 0.300 400 i 2 00 90.0 I0,0 0.0 00 0.300 400 5 00 i0.0 90.0 0.0 00 0.300 400 _ 9 00 i0.0 90.0 0.0 00 0.300 400 9 50 0.0 I00.0 0.0 00 0.300 400 14 00 0.0 100..0 0.0 00 0.300 400 14 50 90.0 i0,0 0.0 00 0.300 400 20.00 90.0 i0.0 0.0 00 0.300 400 _HPll00 LC Pump External Event Timetable The Timetable contains 6 entries which are : Time Initial 0.00 0.05 0.i0 11.90 12.00 Column Switch Off Off Off Off Off Off Contactl Off On Off Off Off Off Contact2 Off Off Off On Off Off Contact3 Off Off Off Off On Off Contact4 Off Off Off Off Off Off HPIIOQ Autosampler Initial Conditions Draw Speed Eject Speed (#i/min) Draw Position (mm) Stop Time (mins) Injection Volume(#l) Vial Number 200.0 200 0.50 20.00 15.0 47 Tuning Method Method: Report C :\MAS SLYNX\FLUOROCHEMICALS. PRO\ACQUDB\FLUOROCHEMS Printed: Wed Aug 13 09:37:50 2003 _I,_I0_ U Page 1 _ Dau 395.00 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Desolvation Temp. Temp. Pressures Analyser Gas Cell Vacuum Set Rdbk 3.00 20 0.0 0.0 0.0 i00 300 -2.93 -42 I00 299 Rdbk OFF 3.5e-3 Analyser LM K_s I 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 26 - 15 38 2 29 14.0 14.0 2.0 650 -648 Rdbk 132.1 755.7 Quantify Calibration Report Study No. _L34910, Set No. :081203A, Ext.Date:08/12/03, Analyst:K.Risha Calibration: Last modified: Pri_ed, P:\Data\LCMSMS6\Masslynx\Fluorochem/cals.PRO\CurveDB\081203A Mon Aug 18 10:47:18 2003 .on*ug18lO,5O:220,03 Compound Iname:C8 Sulfonat(ePFOS) CoefficieonftDeterminatio0n.:998540 Calibration curve: 39.6727 * x + 10.4732 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: l/x, Axis trans: None 3.97e4- Page 1 Decatur BC _._II_(03_t'_ Response- x 0 .... 0.0 _ . . , , _ .... 200.0 i .... _ .... 400.0 L .... I .... 600.0 , .... t.',, 800.0 Exygen Research, 3058 Research Drive, State College, PA 16801 I .... _ng/L 1000.0 i Quantify Calibration Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Calibration: Last modified: Printed: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\081203A Mon Aug 18 10:47:18 2003 Mon Aug 18 10:50:24 2003 Compound 2 name: PFOSA Coefficient of Determination: 0.99812!9 Calibration curve: 150.037 * x + 434.4.55 Response type: External Std, Area Curve type: Linear, Origin: Exclude,Weighting: l/x, Axis trans: None 1.50e5- Page 2 Decatur BC Response- V 0 .... i,,,, L,,,, _ .... , .... ,,,,, i .... _ .... _ .... _ .... ,ng/L 0.0 200.0 400.0 600.0 800.0 1000.0 F-.,_gen Research, 3058 Research Drive, State College, PA 16801 I Quantify Sample Study No.:L34910, Report Set NO.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Page 1 Sample List: Last modified: Method: Last modified: Job Code: Printed: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\081203A Mon Aug 18 10:47:09 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS and Mon Aug ii 09:49:08 2003 _nRia|$ _ Date _i _[0_ _ Mon Aug 18 10:50:25 2003 Run#_l_Kc_Iz_#_'-_c_ Decatur BC PFOSA 081103 -- Name: 081203A-3001 Text : : C8 Sulfonate (PFOS) X0C810280131A03-3-00,01 0Smng(M/Ln,S2txa3n)dard lOOq $ 1M3-RAMugo-f2400C3hLaCn/nMeSls/MESS-14:43:39#6 9.309.58 9.98 11;,21 499>99 t 0.27 1.291, 892.20 3.28 4'01x"4"215.145.80 6"_56"77,.7.398.37 A/'/_(_ _ _A_ 792 i 0' .... ,-",,, _, .'-, , , .... , , Time ! .... _ .... , , I _ [ ,'= i [ _ I 1 I r _ r ", , , { ' '' r'-, { _" I , I _ .... r I [ _ r r ', i _ [ i I , { r i i , _ ' ,'"_f 2.00 4.00 6.00 6.00 10.00 2 : PFOSA XC081103-0, 0 ng/L Standard 081203A-3001 Sm (Mn, 2x3) 100-] 1 -6 2.09 3 24 3 61 . 4.38 %-4 7 "_ 5.89 .uo 8.30 5.28 6.8 7.60 1{I-Aug-200314:43:39 LC/MS/MS #6 MRM of 4 Channels ES- 9.30 498 > 78 A 9.98 10.35 583 11.72 01.,, ,, ,.,.,,, _ .... ,, T-,,, .... , .... ,.,. ,.,., ,., ,-,.,, _-.,.. _ .... , .... 2.00 4.00 6.00 8.00 10.00 Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\081203A Mon Aug 18 10:47:09 2003 P:\Data\LCMSMS6\MasslynxkFluorochemicals.PRO\MethDB\PFOS Mon Aug ii 09:49:08 2003 Printed: Mon Aug 18 10:50:26 2003 Page 2 Decatur BC a_d PFOSA 081103 Name: 081203A-3002 Text : I: C8 Sulfona_e (PFOS) IXC081103-1, 25 ng/L Standard 081203A-3002 Sm (Mn, 2x3) 10 909 9.35j 13-Aug-2003 15:05:11 LC/MS/MS #6 MRM of 4 Channels ES- 5.24e3 499> 99 .... -................................ _ ,', ,", , .... , .... Time 2.00 4.00 6.00 8.00 10.00 2 : PFOSA XC081103-1, 25 ng/L Standard 081203A-3002 Sm (Mn, 2x3) 13-Aug-2003 15:05:11 LC/MS/MS #6 MRM of 4 Channels ES- 9.96 498 > 78 1(i/1 3547_ 1.A79reea4 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslyn_\Fluorochamlcals.PRO\SampleDB\081203A Mon Aug 18 10:47:09 2003 P:kData\LCMSMS6\Masslyr_kFluorochemicals.PROkMethDBkPFOS Mon Aug ii 09:49:08 2003 Printed: Mon Aug 18 10:50:26 2003 Page 3 Decatur BC and PFOSA 081105 Name: 081203A-3003 Text : i: C8 Sulfonate (PFOS) XC081103-2, 50 ng/L Standard 081203A-3003 Sm (Mn, 2x3) 13-Aug-2003 15:26:51 LC/MS/MS #6 I MRM of 4 Channels ES-I 121 i' 0 _ . T-._.-;'T. 2 : PFOSA i 7T_ . 7''- 2.00 ' J .... 4.00 t .... I .... 6.00 , .... , ' ' ' "'' 8.00 ......... 10.00 '' " XC081103-2, 50 ng/ Standard 081203A-3003Sm (Mn, 2x3) 13-Aug-2003 15:26:51 LC/MS/MS #E MRM of 4 ChannelsES- i 9.96 498 > 78_ 11! 0-_-_ 2.00 .... 4.00 ,,. . . _ .... 6.00 _ .... , .... 8.00 ,.76I. , 10.00 , , ,"_. 3T.7im3ee4,Area Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Sample List: Last modified: Method: Last modifiad: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\081203A Mon Aug 18 10:47:09 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS Mon Aug ii 09:_9:08 2003 Printed: Mon Aug 18 IQ:50:26 2003 Page 4 Decatur BC and PFOSA 081103 Name: 081203A-3004 Text : i: C8 Sulfonate (PFOS) XC081103-3, 100 ng/h Standard 081203A-3004 Sm (Mn, 2x3) 9.33 I 13-Aug-2003 15:48:30 LC]MS/MS #6 MRM of 4 Channels ES499 > 99 2.18e4 Area ' ' ' $ .... _ ' [ _ _ ' I r _'' ' I'_; ' I '' _ .... I' ' -- _ 2.00 4.00 6.00 8.00 10.00 Time : PFOSA %,J XC081103-3, 100 ng/h Standard 081203A-3004 Sm (Mn, 2x3) 13-Aug-2003 15:48:30 LC/MS/MS #6 MRM of 4 Channels ES- 9.95 498 > 78 Area 1i0_ 15522_ 7.50e4 i I .... r .... ,,,, ,'_ .... j .... _., ', _ .... , .... _ .... T .... J .... , .... Time 2.00 4.00 6.00 8.00 10.00 _J Exygen Research, 3058 Research Drive, State Collage, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Sample List: Last _odified: Method: Last _odified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\San_leDB\081203A Mon Aug 18 10:47:09 2003 p:\Data\LCMSMS6\MasslynxkFluorochemicals.PRO\MethDBkPFOS Mon Aug Ii 09:49:08 2003 Printed: Mon Aug 18 10:50:26 2003 Page 5 Decatur BC and PFOSA 081103 Name: 081203A-3005 Text : i: C8 Sulfonate (PFOS) XC081103-4, 250 ng/L Standard 081203A-3005 Sm (Mn, 2x3) 13-Aug-2003 16:10:15, LC/MS/MS #6I MRM of 4 ChannelsES- 9.35 499 > 99i 2.00 4.00 6.00 8.00 10.00 2 : PFOSA XC081103-4, 250 ng/L Standard 081203A-3005 Sm (Mn, 2x3) 13-Aug-2003 16:10:15 LC/MS/MS #6 MRM of 4 Channels ES- 9.95 498 > 78 Area 0 _-.... f .... ,,, , , , .... , .... j .... f .... _ .... J .... , .... , .... , .... 2.00 4.00 6.00 8.00 10.00 Time Exygen Research, 3058 Research Drive, State College, PA 16801 ,i i llW Quantify Sample Report Study No. :L34910, Set No.:081203A, Ext.Date:08/12/03, Sample List : Last modified: Method : Last modified: Job Code : P :\Data\LCMSMS6\Masslynx\Fluorochenticals. Mon Aug 18 10:47:09 2003 P :\Data\LCMSMS6 \Masslynx\Fluorochemicals. Mon Aug Ii 09:49:08 2003 Printed: Mon Aug 18 10:50:26 2003 Name: 081203A-3006 Text : I: C8 Sulfonate (PFOS) XC081103-5, 500 ng/L Standard 081203A-3006 Sm (Mn, 2x3) Analyst-K.Risha Page 6 PRO\San_IeDB\081203A Decatur BC PR0\MethDB\PFOS and PFOSA 081103 19165 13-Aug-2003 16:32:0C LC/MS/MS #6 MRM of 4 Channels ES- 1.06e5 Are_ 1_1 0' .... _ .... , .... 2.00 ,',',, , r .... 4.00 2 : PFOSA XC081103-5, 500 ng/L Standard 081203A-3006 Sm (Mn, 2x3) J .... J , , .", 6.00 9.33 1 .... , .... i .... _ .... 8.00 10.00 499 > 99 , .... Time 13-Aug-2003 16:32:0 LC/MS/MS #6 MRM of 4 Channels ES- 9.95 498 > 78 10/1 0 _ .... , ;''' ' I , .... 2.00 [ .... _ .... 4.00 } .... , .... 6.00 [ .... ] .... 8.00 73905_ _ .... ' I I I' r [ .... 10.00 3.53e5Area Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify sample Study No.:L34910, Report Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\081203A Mon Aug 18 10:47:09 2003 P:\Data\LCMSMS6kMasslynx\Fluorochemicals.PRO\MethDB\PFOS Mon Aug ii 09:49:08 2003 Printed: Mon Aug 18 10:50:26 2003 Page 7 Decatur BC and PFOSA Q81103 Name: 081203A-3007 Text : i: C8 Sulfonate (PFOS) XC081103-6, 1000 ng]h Standard 081203A-3007 Sm (Mn, 2x3) 13-Aug-2003 16:53:41 LC/MS/MS #6 MRM of 4 Channels ES- 9.33 499 > 99 Area .... i .... _ .... I .... I .... 2.00 4.00 2: PFOSA XC081103-6, 1000 ng/L Standard 081203A-3007Sm (Mn,2x3/ ] .... _ .... 6.00 [ .... ' .... 8.00 [ .... I .... 10.00 , .... Time 13-Aug-2003 16:53:41 LC/MS/MS #6 MRM of 4 ChannelsES- 9.96 498 > 78 Area 11! '' ' ' ' ' .... _ .... 2.00 ' .... _ "" "' _ .... ' .... ' .... r' ' ' , ,14..5..023__ , =. , , . ,-.- 6T.9im1e5 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16841 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\081203A Mon Aug 18 10:47:09 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS Men Aug ii 09:49:08 2003 Printed: Mon Aug 18 10:50:26 2003 Page 8 Decatur BC and PFOSA 081103 Name: 081203A-3008 Text : i: C8 Sulfa_a_e Methanol Wash (PFOSI 081203A-3008 Sm (Mn, 2x3) 13-Aug-2003 17:15:2_ MRM of 4LCh/ManSn/MelSsE#S6- 10_ 0.13 0.98 1.87 2.61 3.26 ./'3 72 4.795.03 5,91 6.80 8"0\ 8 8.90.. 93_2 9.A6^5 /'1_A0.47 11/_.23 499 >94949 , 2.00 2 : PFOSA Methanol Wash 081203A-3008 Sm (Mn, 2x3) /0.12 L>./ tf08,65 100 _0,751.004.=:A % 1.97 ''''_" 4.00 3.71 6.00 8,00 10,00 5426.14- ! l_-Aug-2003 17:15:2_ =1 LC/MS/MS #6 MFIMof 4 ChannelsES- 9 39 9.98 498 > 78 - 7.17 7.53 8.24 8.9"A9 _ 10.72 11.57 ,,78579 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No.:L34910, Report Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\DatakLCMSMS6\MasslynxkFluorochemicals.PR0kSampleDBk081203A Mon Aug 18 10:47:09 2003 P:kData\LCMSMS6\Masslynx\Fluoxochemicals.PRO\MethDB\PFOS Mon Aug ii 09:49:08 2003 Printed: Mon Aug 18 10:50:26 2003 Page 9 Decatur BC and PFOSA 081103 Name: 081203A-3009 Text : i: C8 Su!fonate Reagent Blank (PFOS) 13-Aug-2003 17:36:58_ f 081203A-3009 Sm (Mn, 2x3) 100 9.13118 3.34__. _0.47 " 2.1 2.35 0 3.74 4.71 5.42 5.63 7.41 8.0 MRM of 4LC/hMaSn/nMeSls ES#6- 1t 11 0611"86"499 > 99 842 . 79.509.78 .\ A 738J ' O .... J .... J .... 2,00 J , ," , t' } , [-,'r' 4.00 '] .... J .... 6.00 J'' ' , ,, , ,-_ ,_ .... 8.00 , , ,,, 10.00 , .... Time _I_ 2 : PFOSA Reagent Blank 081203A-3009 Sm (Mn, 2x3) ,,,, uu-_0.10 2 27 " 7 1"21211 A__^3.373.65 4_o523_^_ | 1,_TAug'2003 17:36:5_ _' LC/MS/MS #6 MRM of 4 Channels ES- 8 56 9 93 .... 498 > 78 . _u.o_ =_A _,_,,824_ 8.78 = xA A 11161141 591 0-_, , . _ , .. , _-., , , , _ , , _ .... 2.00 4.00 _ .... _ , , , , _ .... i .... 6.00 8.00 t , , ,., _ .... 10.00 t--, . , , Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Axlalyst:K.Risha SamDle List: Last modified: Method: Last modified: Job Code: P:kData\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\081203A Mon Aug 18 10:47:09 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS Mon Aug ii 09:49:08 2003 Printed: Mon Aug 18 10:50:26 2003 Page i0 Decatur BC and PFOSA 081103 Name: 081203A-3010 Text : i: C8 Sulfonate (PFOS) _Spk A, 50 ng/L 081203A-3010Sm (Mn,2x3) 13-Aug-2003 17:58:42 LC/MS/MS #6 MRM of 4 Channels ES- 9.33 499 > 9g Area, 0.',, , , r .... _.... 2.00 , .... J .... 4.00 2 : PFOSA Reagent Spk A, 50 ng/L 081203A-3010 Sm (Mn, 2x3) ,., ,, ,,, ,.,,, .... _ .... , .... , .... 6.00 8.00 10.00 , , , , , Time 13-Aug-2003 17:58:42 LC/MS/MS #6 MRM of 4 Channels ES- 9.96 498 > 78 1(ii 1 0 "l ; "I .......... J I_ 2.00 '_ ' "'_'' _ --' 4.00 _" "';'''" _ '"' _--_--T'-' - ' _'' ' ' ' _ ..7..21. _ '' : _ '' " :'--3T.5im7ee4Area 6.00 8.00 10.00 Exygen Research, 3058 Research Driva, State College, PA 168QI Quantify Seu_le Study No.:L34910, Re_ort Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDBk081203A Mon Aug 18 10:47:09 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PROkMethDB\PFOS Mon Aug ii 09:49:08 2003 Printed: Mon Aug 18 10:50:26 2003 Page Ii Decatur BC and PFOSA 081103 Name: Text: 081203A-3011 i: C8 Sulfonate (PFOS) Reagent Spk B, 500 ng/L 081203A-3011Sm (Mn,2x3) 13-Aug-2003 18:20:23 LC/MS/MS #6 MRM of 4 ChannelsES- 9.36 499 > 99 0 t .... _ .... _ ,,,, 2.00 _ .... _ .... 4.00 2: PFOSA iReagent Spk B, 500 ng/L 081203A-3011 Sm (Mn, 2x3) _ .... _ .... 8.00 _ .... _ .... 8.00 _ .... '_ .... _ .... 10.00 Time 13-Aug-2003 18:20:23 LC/MS/MS #6 MRM of 4 ChannelsES- 9.97 498 > 78 0 I .... , .... I .... I .... , .... _ .... , "' ' ' , .... I .... , .... I .... i .... 2.00 4.00 6.00 8.00 10.00 Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Senile List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDBk081203A Mon Aug 18 i0:47:09 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS Mon Aug 11 09:49:08 2003 Printed: Mon Aug 18 10:50:26 2003 Page 12 Decatur BC and PFOSA 081103 Name: 081203A-3012 Text : i: C8 Sulfonate (PFOS) 534910-11 Spk E, 100000 ng/L, DF=1000 081203A-3012 Sm (Mn, 2x3) 13-Aug-2003 18:42:04 LC/MS/MS #6 MRM of 4 Channels ES- 9.35 499 > 99 1i_ 2.00 4.00 %,# 2 : PFOSA 534910-11 Spk E,100000 ng/L,DF=1000 6.00 081203A-3012 Sm (Mn, 2x3) 85411 8.00 10.00 4.55e4Area 13-Aug-2003 18:42:04 LC/MS/MS #6 MRM of 4 ChannelsES- 9.98 498 > 78 i1 - 1i_ 11415_ 5.2A3ree4a , , , _ .... "t, , , , _ .... _ , , , ' _ .... _"" ' ' _ .... _ .... 2.00 4.00 6.00 8.00 Y.... i ' ,', , _ .... 10.00 Time Exygen Research, 3058 Research Drive, State College, PA 16801 |I Quantify sample Study No.:L34910, Report Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDB\081203A Mon Aug 18 10:47:09 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PRO\MethDB\PFOS Mon Aug ii 09:49:08 2003 Printed: Mon Aug 18 10:50:26 2003 Page 13 Decatur BC axld PFOSA 081103 Name: 081203A-3013 Text : i: C8 Sulfonate (PFOS) L34910-11 Spk E, 100000 ng/L, DF=100 081203A-3013 Sm (Mn, 2x3) 13-Aug-2003 19:03:40 LC/MS/MS #6 MRM of 4 ChannelsES- 9.36 499 > 99 0 _.... , .... , .... 2.00 , .... ', ,", < , , .... ,'-,,,,, 4.00 6.00 .... , .... 8.00 , .... , .... 10.00 ,, ,-, , Time 2 : PFOSA _ L34910-11 Spk E, 100000 ng/h, DF=100 081203A-3013 Sm (Mn, 2x3) 13-Aug-2003 19:03:40 LC/MS/MS #6 MRM of 4 ChannelsES- 9.98 498 > 78 0 I'' ' ' ' , .... , .... 2.00 _ .... 'L .... 4,00 J .... , .... 6.00 J .... , .... 8.00 , .... t''' " , .... 10.00 Time Exygen Research, 3058 Research Drive, State College, PA 16801 I i| Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, AnalySt:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDBk081203A Mon Aug 18 10:47:09 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS Mon Aug ii 09:49:08 2003 Printed: Mon Aug 18 10:50:26 2003 Page 14 Decatur BC and PFOSA 081103 Name: 081203A-3014 Text : i: C8 Sulfonate (PFOS) XC081103-1, 25 ng/L Standard 081203A-3014 Sm (Mn,2x3) 13-Aug-2003 19:25:25_ LC/MS/MS #6 I MRM of 4 Channels ES-[ 9.36 499 > 99] ,/= ........ _ .... 2.00 , '' '-"_', "_' ' 4.00 i .... , .... 6.00 ___ ,. _ , , , _ .... _ , ,', , , .... 8.00 10.00 Area Time 2 : PFOSA XC081103-1, 25 ng/L Standard 081203A-3014 Sm (Mn,2x3) 13-Aug-2003 19:25:25 LC/MS/MS #6 MRM of 4 Channels ES- 9.96 498 > 78 1(_/l 0 _''--_, , .... , .... 2.00 J .... r-_, , . , .... , .... 4.00 6.00 , . ' ' ' , .... 8.00 423__L , .... c' 10.00 2.1A0re4a -"' , ,_Time V Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6kMasslynx\Fluorochemlcals.PRO\Sam_leDBk081203A Mon Aug 18 10:47:09 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS Mon Aug ii 09:49:08 2003 Printed: Mon Aug 18 10:50:26 2003 Page 15 Decatur BC and PFOSA 081103 Name: 081203A-3015 Text : i: C8 Sulfonate (PFOS) XC081103-2, 50 ng/L Standard 081203A-3015 Srn (Mn, 2x3) 13-Aug-2003 19:47:12 LC/MS/MS #6 MRM of 4 ChannelsES- 2208- 1.24e4 Area i lol 9.3, 499,99 ! 0_ .... J ,,'-,, .... 2.00 , .... , .... 4.00 J, ,,',,..,, 6.00 i .... i, .,-_,;-T'_...... ., ..... 8.00 10.00 Time 2 : PFOSA XC081103-2, 50 ng/L Standard 081203A-3015 Sm (Mn, 2x3) 13-Aug-2003 19:47:12 LC/MS/MS #6 MRM of 4 ChannelsES- 0!1 0 _' ' ' "1-'-' ' ' _ .... 2.00 819 3.75e4 Area , .... I ' '-' I .... I ' '_" I .... i',_--, , _ .... I ' _""'1 '-"" Time 4.00 6.00 8.00 10.00 ';l,J Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, ',_ Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\081203A Mon Aug 18 10:47:09 2003 P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\MethDB\PFOS Mon Aug Ii 09:49:08 2003 Printed: Mon Aug 18 10:50:26 2003 Page 16 Decatur BC and PFOSA 081105 Name: 081203A-3016 Text : i: C8 Sulfonate (PFOS) XC081103-3, 100 ng/L Standard 081203A-3016 Sm (Mn,2x3) 13-Aug-2003 20:08:51 LC/MS/MS #6 MRM of 4 Channels ES- 9.36 499 > 99 1(i/l 2.00 4.00 6.00 8.00 4213L 10.00 T2i.m30ee4Area 1 0 _ .... I .... J .... , .... , ,', I r [ .... | .... J .... I .... ' .... } .... , .... 2 : PFOSA XC081103-3, I00 ng/L Standard 081203A-3016 Sm (Mn,2x3) 13-Aug-2003 20:08:51 LC/MS/MS #6 MRM of 4 Channels ES- 9.96 498 > 78 1i_ __ .... J .... , '" r , r _ .... 2.00 _ .... 4.00 _ .... , .... 6.00 16248_ , .... , r , , _ , ; , , , , .... 8.00 10.00 7.75e4Area ,_ , , Time q',Jl_ Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify San_le Report Study No.:L34910, Set No.:081203A, Ext. Date:08/12/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\081203A Men Aug 18 10:47:09 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PPOS Men Aug ii 09:49:08 2003 Printed: Men Aug 18 10:50:26 2003 Page 17 Decatur BC and PFOSA 081103 Name: 881203A-3017 Text : i: C8 Sulfonate (PFOS) L34910-11, DF=1000 081203A-3017Srn (Mn,2x3) 13-Aug-2003 20:30:3..: LC/MS/MS #6 MRM of 4 ChannelsES- 9.35 499 > 99 Area i 10_0-__, , , , ,.... _ .... 2.00 2 : PFOSA qi,,' L34910-11, DF=1000 ,, ,., , j , , ,,, _ .... ,.... 4.00 6.00 081203A-3017 Sm (Mn, 2x3) _ .... , .... 437,8_,.,, , _', ,-,, _, _'_-T2-,T.3im9ee4 8.00 10.00 13-Aug-2003 20:30:3._ LC/MS/MS #E MRM of 4 Channels ES- 9.95 498 > 78; 0 I .... E.... r .... 2.00 i .... = .... 4,00 i .... i,,,, 6.00 i .... -, .... 8.00 _._ f .... i .... , i .... 10.00 Area -Time Exygen Research, 3058 Research Drive, State College, PA 16801 I Quantify SaE_le Study No.:L34910, Report Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemlcals.PR0\Sam_leDB\081203A Mon Aug 18 10:47:09 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS Mon Aug ii 09:49:08 2003 Printed: Mon Aug 18 10:50:26 2003 Page 18 Decatur BC and PFOSA 081103 Name: Q81203A-3018 Text : i: C8 SulfonaZe (PFOS) L34910-11 Rep, DF=1000 081203A-3018 Sm (Mn, 2x3) 13-Aug-2003 20:52:1 LC/MS/MS #E MRM of 4 Channels ES- Area 1 i 0_-_--_., .... J .__-r .... J .... ,'.,., _ ,-. ,,. r--_,.,,.,,,, 2.74e4 .... , .... _Time 2.00 4.00 6.00 8.00 10.00 2 : PFOSA 534910-11 Rep, DF=I000 081203A-3018 Sm (Mn, 2x3) 13-Aug-2003 20:52:12 LC/MS/MS #6 MRM of 4 Channels ES- 9.96 498 > 78 _L 0 I .... , .... , .,,, _ .... f .... , . . . , , ,-.. T i .... ,"r, ,,, ,, . , i .... _ .... 2.00 4.00 6.00 8.00 10.00 Area Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Re_ort _r Study No.:L34910, Set No.:081203A, Ext.Date:08112/03, Analys_:K.Risha San_le List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochamicals.PRO\Sam_leDB\081203A Mon Aug 18 10:47:09 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS Mon Aug ii 09:49:08 2003 Printed: Mon Aug 18 10:50:26 2003 Page 19 Decatur BC and PFOSA 081103 Name: 081203A-3019 Text : i: C8 Sulfonate (PFOS) L34910-11, DF=100 " 081203A-3019 Sm (Mn, 2x3) " ... - .,'-- 13-Aug-2003 21:13:55 LC/MS/MS #E MRM of 4 Channels ES- 9.34 499 > 99 1i 0 _.... ._T-, . . _ .... 2.00 2 : PFOSA !L34910-11, DF=100 , .... , .... 4.00 081203A-3019 Sm (Mn, 2x3) _ .... , .... 6.00 422196 2.24e Area ! , .... , .... .., .... "1.... , .... 8.00 10.00 Time 13-Aug-2003 21:13:55 LC/MS/MS #6 MRM of 4 Channels ES- 9.96 498 > 78 11/1 0 _r ' ' j l " ' ' , .... 2.00 J .... ) .... 4.00 , .... , .... 6.00 , .... [ .... 8.00 13834_ _ .... _ ' ' ' '' 10.00 _ .... 6.48e4Area Time Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L34910, Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\Sam_leDBk081203A Won Aug 18 10:7:09 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PFOS Mon Aug ii 09:49:08 2003 Printed: Mon Aug 18 10:50:26 2003 Page 20 Decatur BC and PFOSA 081103 Name: 081203A-3020 Text : I: C8 Sulfonate (PFOS) L34910-11 Rep, DF=100 081203A-3020 Sm (Mn, 2x3) 13-Aug-2003 21:35:42 LC/MS/MS #6i MRM of 4 Channels ES- 9.36 499 > 99 11o/1 2.00 4.00 6.00 8.00 483561 10.00 2T.5im1ee5Area _' 0 I .... " , .... ] .... I r , ', , l .... J .... r _' '''I .... ] "' ' ' ' ' .... I .... , r ,", r 2 : PFOSA L34910-11 Rep, DF=100 081203A-3020 Sm (Mn, 2x3) 13-Aug-2003 21:35:42 LC/MS/MS #6 ' MRM of 4 ChannelsES- 9.98 498 > 78 2.00 4.00 6.00 8.00 10.00 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Study No0:L34910, Report Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMSe\Masslynx\Fluorochemicals.PRO\Sam_leDB\081203A Mon Aug 18 10:47:09 2003 P:\Data\LCMSMSe\Masslynx\Fluorochemicals.PRO\MethDB\PFOS Mon Aug Ii 09:49:08 2003 Printed: Mon Aug 18 10:50:26 2003 Page 21 Decatur BC and PFOSA 081103 Name: 081203A-3021 Text : i: C8 Sulfonate (PFOSI XC081103-4, 250 ngJL Standard 081203A-3021Sm (Mn,2x3) 13-Aug-2003 21:57:23 LC/MS/MS #6 MRM of 4 ChannelsES- 9.36 499 > 99 11o/1 110391 5.8A5re8a4 t 0_,, , . j .... _ .... , ,, , , 1 .... , .... _ .... -_ .... _ .... ,_ , , , , , ,', _ , , , Time 2.00 4.00 6.00 8.00 10.00 2 : PFOSA !XC081103-4,250 n_L Standard 081203A-3021Sm (Mn,2x3) 13-Aug-2003 21:57:2_. LC/MS/MS #6 MRM of 4 ChannelsES- 9.98 498 > 78 Area 10o0_I 411221 2.00 4.00 6.00 8.00 10.00 1.97e5 Exygen Research, 3058 Research Drive, State College, PA 16801 I II Quantify San_le Study No.:L34910, Report Set No.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:kDa_akLCMSMS6\Masslynx\Fluorochemicals.PROkSam_leDB\081203A Mon Aug 18 10:47:09 2003 P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOS Mon Aug Ii O9:49:08 2003 Printed: Mon Aug 18 10:50:26 2Q03 Page 22 Decatur BC and PFOSA 081103 Name: 081203A-3022 Text : i: C8 Sulfonate (PFOS) XC081103-5, 500 ng/L Standard 081203A-3022 Sm (Mn, 2x3) 13-Aug-2003 22:19:08_ LC/MS/MS #6 I MRM of 4 Channels ES- t 9.35 499 > 991 1i0_ 20668_ 1.09e51Area t 2.00 4.00 6.00 8.00 10.00 _m_ 2: PFOSA XC081103-5,500 ng/l Standard 081203A-3022 Sm (Mn, 2x3) 13-Aug-2003 22:19:08 LC/MS/MS #6 MRM of 4 ChannelsES- 9.96 498 > 78 1i_ 0 _ .... ,I I '= '1 ', .... 2.00 _ .... , ' [' ' '' 4.00 [ ' I "-- ' T .... 6.00 , .... , .... 8.00 78848_ j .... J .... 10.00 j .... 3.74e5Area Time Exygen Research, 3058 Research Drive, State College, PA 16801 S I II, Quantify Sample Study No.:L34910, ReDort Set NO.:081203A, Ext.Date:08/12/03, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\San_leDB\081203A Mon Aug 18 10:47:09 2003 P:\Data\LC14SMS6\Masslynx\_luorochemicals.PRO\MethDB\PFOS Mon Aug ii 09:49:08 2003 Printed: Mon Aug 18 10:50:25 2003 Page 23 Decatur BC and PFOSA 081103 Name: 081203A-3023 Text : i: C8 Sulfonate (PFOS) XC081103-6, 1000 ng/L Standard 081203A-3023 Sm (Mn, 2x3) 39291 13-Aug-2003 22:40:47_ MRM of 4LCCh/ManSn/MelSs E#S6- I 2.13e5 Area 0''' '''' ' ] .... ] .... 2.00 _ .... ] .... 4.00 2 : PFOSA XC081103-6, 1000 ng/L Standard 081203A-3023 Sm (Mn, 2x3) ] .... _ .... 6.00 8.00 ,",, 10_.00 ' .... I ] 1 ' .... .... , .... Time 13-Aug-2003 22:40:47_ LC/MS/MS #6 I MRM of 4 Channels ES-[ 9.96 498 > 78I 1i_ __ .... _ .... j .... 2.00 149443_ 7.03e5Area J .... ' T' I " ' ] .... 4.00 I "' ' r'' 6.00 , .... , [ ' '-,-, 8.00 .... _ .... _ .... 10.00 Time Exygen Research, 3058 Research Drive, State College, PA 16801 ii Ill II 9/19/2003 Project: E03-0561 35'I ENVIRONMENTAL LABORATORY b_-ml Report 1 of 3 Requester: Schnobrich, Dana M (223-1N-08) Department: 530711 Project Number: 0022674449 Date Received: 6/26/2003 Project Description: Decatur Bakers Creek #2 Surface Water and Sediment Comments: Completion Date: 9/2/2003 Project Lead: Jess S. Eldridge Phone Number: 651-778-5233 Email Address: jseldridge@mmm.com Statement of Accuracy: Based on results of field spikes, laboratory spikes, field blank spikes, and laboratory control spikes, the analytical accuracy for all compounds is 30%. Exceptions for the water samples are as follows: BC2 SW-04 high spike (PFOA 57%, PFOS - 62%, FOSA - 58%), BC2 SW-05 high spike (PFOA - 66%, FOSA - 40%), BC2 SW-06 high spike (FOSA - 60%), Outfall to River SW-25 (FOSA - 58%). Also, several low spike samples showed unacceptable recoveries in cases where the spiking concentration was comparable or below the inherent sample concentration. However, all laboratory control spikes, laboratory matrix spikes, and all other field spikes showed recoveries between 70% and 130% for all compounds. The accuracy for the sediment samples is based upon laboratory spike recoveries, all of which were between 70% and 130% for all compounds. Sediment sample results are reported as received. Results reported as dry weight are available in the Exygen report. I REVISED REPORT: Due to schedule changes, the original sample dates entered were revised to relect the actual collection dates. BGJ-Pace-9/I 9/03 Pr o_itResu|tslActivi_ Pace Field Sampling Event - Complete 3M Smnple Number E03-0561-49786 Sampled Date 7/21/2003 EXYGEN EXYGEN EXYGEN EXYGEN E03-0561-49787 Analytical Methg_] PFOS by ESMS PFHS FOSA PFOA 9/21/2003 LAB Analytical Method EXYGEbl PFOS by ESM5 EXYGEN PFHS EXYGEN FOSA EXYGEN PFOA E03-0561-49788 7/23/2003 LAB A_d.T_c.IJ..._,_ EXYGEN PFOS by ESMS EXYGEN PFHS EXYGEN FOSA ExryGEN PFOA E03-0561-49789 7/21/2003 LAB EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS Sample Description BC2 SW-04 Comnonents PFOS PFHS FOSA PFOA BC2 SW-04 DUP _:omoonents PFOS PFHS FOSA PFOA BC2 SED-04 Comoonents PFOS PFHS FOSA PFOA BE1 SW-05 Component_ PFOS PFHS Result RL 11.5 ng/mL 0.05 0.896 ng/mL 0.05 1.39 ng/mL 0.05 4.21 ng/mL 0.05 Result RL 8.25 ng/mL 0.05 0.571 ng/mL 0.05 0.790 ng/mL 0.05 2.54 ng/mL 0.05 Result RL 14.6 ng/g 0.4 0.566 ng/g 0.4 7.15 ng/g 0,4 3.02 nglg 0.4 Result RL 1.67 ng/mL 0.05 O.155 ng/mL 0.05 9/19/2003 3M KNVIRONMENTAL LABORATORY Final Report 2 of 3 Project: E03-0561 (cont.) 3M Sample Number E03-0561-49789 (cont.) Sampled Date 7/21/2003 Sample Descripfon BC2 SW-05 LAB EXYGEN EXYGEN E03-0561-49790 Analytical FOSA PFOA Method 7/21/2003 Comaonents FOSA PFOA BC2 SW-05 DUP Result RL 0.146 ng/mL 0.05 0.591 ng/mL 0.05 LAB EXYGEN EXYGEN EXYGEN EXYGEN E03-0561-49791 Analytical Method PFOS by ESMS PFHS FOSA PFOA 7/21/2003 Qomugnents PFO S PFH S FOSA PFOA BC2 SED-05 Result RL 4.33 ng/mL 0.05 0.377 ng/mL 0.05 0.389 ng/rnL 0.05 1.56 ng/mL 0.05 LAB Analytical Method Comoonents Result RL EXYGEN PFOS by ESMS PFOS 22.8 ng/g 0.4 1 EXYGEN PFHS PFHS 1.45 ng/g 0.4 ] EXYGEN FOSA FOSA 7.86 ng/g 0.4 EXYGEN PFOA PFOA 5.14 ng/g 0.4 E03-0561-49792 7/23/2003 BC2 SW-06 LAB EXYGEN EXYGEN EXYGEN EXYGEN E03-0561-49793 Analytical Method PFOS by ESMS PFHS FOSA PFOA 7/23/2003 Comnonents PFOS PFHS FOSA PFOA BC2 SW-06 DUP Result RL 26.1 ng/mL 0.05 6.06 ng/mL 0.05 2.43 ng/mL 0.05 12.1 ng/mL 0.05 LAB EXYGEN EXYGEN EXYGEN EXYGEN E03-0561-49794 _ PFOS by ESMS PFHS FOSA PFOA 7/23/2003 Comnonents PFOS PFHS FOSA PFOA BC2 SED-06 Result RL 25.1 ng/mL 0.05 5.87 ng/mL 0.05 2.57 ng/mL 0.05 11.6 ng/mL 0.05 LAB EXYGEN Analytical Method PFOS by ESMS C'omoonents PFOS Result RL 880 ng/g 0.4 EXYGEN EXYGEN PFHS FOSA PFHS FOSA 2.46 ng/g 0.4 71.4 ng/g 0.4 EXYGEN E03-0561-49795 PFOA 7/23/2003 PFOA Ouffall to River SW-25 14.2 ngtg 0.4 LAB Analytical Method _'omDonents Result RL EXYGEN PFOS by ESMS PFOS 31.2 ng/mL 0.05 EXYGEN PFHS PFHS 7.66 ng/mL 0.05 EXYGEN FOSA FOSA 3.26 ng/mL 0.05 EXYGEN PFOA P FOA 15.8 ng/mL 0.05 E03-1_561-49796 7/23/2003 Ouffall to River SW-25 DUP LAB EXYGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA _ PFOS PFHS FOSA Result 30.8 ng/mL 6.77 ng/mL 3.28 ng/mL " RL 0.05 0.05 0.05 9/19/2003 354 E/WIRONMENTAL LABORATORY Final Report 3 of 3 Project: E03-0561 (cont.) 3M Sample Number E03-0561-49796 (cont.) Sampled Date 7/23/2003 Sample Description Ouffall to River SW-25 DUP LAB EXYGEN E03-0561-49797 Analytical PFOA Method 7/23/2003 Comoonfnts PFOA OuffaH To River SED-25 Result RL 14.4 ng/rnL 0.05 LAB Analytical Method Comnoq_nts Result RL EXYGEN PFOS by ESMS PFOS 107 ng/g 0,4 EXYGEN PFH S PFH S 3.19 ng/g 0,4 EXYGEN FOSA FOSA 28,0 ng/g 0.4 ! EXYGEN PFOA PFOA 10,7 ng/g 0.4 E03-0561-49813 7/23/2003 Outfall to River SED-25 DUP LAB EXYGEN Analytical Method PFOS by ESMS _ PFOS Result RL 140 ng/g 0.4 EXYGEN PFHS PFHS 4.98 ng/g 0.4 EXYGEN FOSA FOSA 35.7 ng/g 0.4 j EXYGEN PFOA PFOA 17.7 ng/g 0.4 E03-0561-59479 7/21/2003 Field Control/Travel Blank LAB _ Comoonents Result RL EXYGEN PFOS by ESMS PFOS ND ng/mL 0.05 EXYGEN EXYGEN PFHS FOSA PFHS FOSA ND ng/mL 0.05 ND ng/mL 0.05 EXYGEN PFOA PFOA ND ng/mL 0.05 E03-0561-59480 7/21/2003 Equipment Blank - Pump LAB Analytical M_thod Component| Result RL EXYGEN PFOS by ESMS PFOS ND ng/mL 0.05 EXYGEN PFHS PFHS ND ng/mL 0.05 EXYGEN EXYGEN FOSA PFOA FOSA PFOA bid ng/mL 0.05 ND ng/mL 0.05 E03-0561-59481 7/21/2003 Equipment Blank - Dredge LAB EXYGEN EX'YGEN EXYGEN EXYGEN Analytical Method PFOS by ESMS PFHS FOSA PFOA Comoonent$ PFOS PFHS FOSA PFOA Result ILL ND ng/mL 0.05 ND ng/mL 0.05 ND ng/mL 0,05 ND ng/mL 0.05 Project Lead Review: _'S_f_5 Date: _/[ _/O