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AR A * 6 - / 7 / 0 Proven Results. f ti 11 Analytical Report f* Fluorochemical Characterization of Water Samples Daikin America, Inc. Exygeh Research Laboratory Report No. L0001297 nS 4 nI.! Testing Laboratory Exygen Research 3058 Research Drive State College, PA 16801 PI I- 4 Requester N> Randy Roussel Daikin America, Inc. PO Box 2252 Decatur, AL 35609 TJ'&Y*} x> ro --i o-o rzno ~--o\op t -ZXS)i cP pn o F3 M* JI IP"? p\ n Is-i 000283 3 0 5 8 Research Drive State College, PA 16 8 01 , USA PAGE J: 800.281.3219 F: 8 1 4 .2 7 2 .1 0 1 9 exygen.com ";'Y Introduction ;:: si^s -;fife . ': ; ,: r"':M :JY .V ' A,':. ZSAVZ'Aa. A:A A .1 Results are reported for the analysis of surface water and sediment samples received by Exygen Research (Exygen) from Daikin America. The Exygen study number assigned to the project is L0001297. Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC/M S/M S) was requested for all samples. A total of 1 sample was received for analysis. T h e samples was prepared and analyzed by LC/MS/M S for the following list of fluorochemicals: Table 1: T arget Analysis Compound Name Perfluorooctanoic Acid Acronym C8 Acid (PFOA) T he analytical methods used were originally developed for groundwater samples and were validated by Exygen. The validation protocol and results are on file with Exygen. Sample 'm m T h e sample was submitted in a plastic container. All samples were cooled to 4C from time of collection to receipt at Exygen Research. Samples were stored at 4C from receipt at Exygen Research until analysis. Samples were collected on 11/11/03. 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 3 0 days of receipt. 4 Methods - Ana, :JA Z .:i^ ' ;- separatory 4.1 LC/MS/MS 4.1.1 Sample Preparation for LC/MS/MS Analysis Samples were initially treated with 200 uL of 250 mg/L sodium thiosulfate solution to remove residual chlorine. Solid phase extraction (SPE) was used to prepare the samples for LC/M S/M S analysis. A forty-milliliter portion of sample was used for analysis. The samples were transferred to a C i8 SPE cartridge. The cartridge was eluted with 5 mL of 100% methanol. This treatment resulted in an eight-fold concentration of the diluted samples prior to analysis. PAGE2 OF5 000284 4.1.2 Sample Analysis by LC/MS/MS In HPLC, an aliquot of extract is injected and passed through a liquid-phase chromatographic column. Based on the affinity of the analyte for the stationary phase in the column relative to the liquid mobile phase, the analyte is retained for a characteristic amount of time. Following HPLC separation, ES/M S provides a rapid and accurate means for analyzing a wide range of organic compounds, including fluorochemicals. Electrospray is generally operated at relatively mild temperatures; molecules are ionized, fragmented, and detected. Ions characteristic of known fluorochemicals are observed and quantitated against standards. A Hewlett-Packard H P 1100 H PLC system coupled to a Micromass Ultima M S /M S was used to analyze the sample extracts. Analysis was performed using selected reaction monitoring (SRM ). Samples extractions and analyses were performed on 11/17/03 and 11/24/03. Exact dates for extraction and analysis of each sample batch are given in the raw data. Raw analytical data is provided in Attachment D. 5 Analysis 5.1 5.2 5.3 5.4 Calibration A 7-point calibration curve was analyzed at the beginning and end of the analytical sequence for the compounds of interest. The calibration points were prepared at 0, 25, 50, 100, 250, 500, and 1000 ng/L (ppt) for LC/MS/MS analysis. The instrument response versus the concentration was plotted for each point. Using linear regression with 1/x weighting, the slope, y-intercept and correlation coefficient (r) and coefficient of determination (r2) were determined. A calibration curve is acceptable if r >.0.985 (r2 > 0.970). Calibration standards are prepared using the same SPE procedure used for samples. Calibration check standards were analyzed periodically (every three to five sample injections) throughout the analysis sequence. Compliance is obtained if the standard analyte concentrations are within +/-20% of the actual value. All calibration criteria were met for this analysis. Blanks Extraction blanks were prepared and analyzed with every extraction batch of samples. The extraction blanks should not have any target analytes present at or above the concentration of the low-level calibration standard. For these samples, the extraction blanks w ere compliant. Instrument blanks in the form of clean methanol solvent were also analyzed after every highlevel calibration standard, and after known high-level samples. Again, the blanks should not have any target analytes present at or above the low-level calibration standard. For the samples presented here the instrument blanks are compliant. Surrogates Surrogate spikes are not a component of the LC/MS/M S analytical methods. Matrix Spikes Matrix spikes were prepared for each sample. Matrix spike recoveries are given in Attachment B. 000ZS5PAGE3 OF5 5.5 Duplicates Laboratory duplicates were performed for each sample. The duplicate results are included with the sample results In Attachment A. 5.6 Laboratory Control Samples For LC/M S/M S analyses, Milliq water was spiked with all compounds with each extraction set. All recoveries for all compounds were between 70-130% in each LCS. Results are given along with the raw data in Attachment D. Please see Attachment A for a detailed listing of the analytical results. Results are reported in units of parts per million (ppm) (ug/mL). Samples are disposed of one month after the report is issued unless otherwise specified. All electronic data is archived on retrievable media and hard copy reports are stored in data folders maintained by Exygen. 8.1 Attachment A: Results 8.2 Attachment B: Matrix Spike Recoveries 8.3 Attachment C: Chain of Custody 8.4 Attachment D: R aw Analytical Data PAGE 4 OF5 000286 9 Signatures Other Lab Members Contributing to Data Karen Risha 000287P A G E 5 0 F 5 n 4?V. - p Proven Results. t' !; i.J Summary of PFOA in W ater Samples f ri Analyte Found (pg/mL) Sample ID______ PFOA DSN001 ~ D SN 001*__________________ 03 1.10 *l :i t 3 ` Laboratory Duplicate * -i : fi H U t- u 00028S v V ^ k 3 0 5 8 Research Drive * m S t a t e College, PA 16 8 01 , USA r 814.272.1039 F : 814.231.1580 exygen.com STANDARD TERMS AND CONDITIONS Services provided by Exygen Research are limited to the terms and conditions stated herein, unless otherwise agreed to in a formal contract. CONFIDENTIALITY-- Exygen Research ("Exygen," "us," or "w e") maintains the strictest confidentiality in all of our client interactions. If a signed confidentiality agreement is required, we will provide one. If a regulatory or legal body subpoenas information, the client will be notified promptly. The client agrees not to use Exygen's name and/or data in any manner that might cause harm to Exygen's reputation or business. Approval must be obtained, in writing, before Exygen's name can be published in any way. CONTRACTS--AW contracts are subject to review and approval by Exygen's legal council and must be signed by a corporate officer. PAYMENT TERMS-- Unless otherwise set forth in this Purchase Order, terms of payment are "N et 30 Days." The time allowable for payment shall begin after both: (a) client's receipt o f Exygen's invoice; and (b) the satisfactory performance of the services contemplated hereunder. A 1.5% monthly service charge shall be added to all past due balances. 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All samples submitted must be accompanied by: purchase order, or signed quotation; sample description, including sample type, source, time and date of collection; specific analyses requested; estimated concentration levels; requested report date; current billing address; and other relevant information. Upon request, Exygen will provide and ship appropriate sample containers to clients. These containers will include the appropriate preservative if particular analyses *-equire one. It is the responsibility of the client to handle these preserved containers safely, and using all appropriate safety precautions. Clients requesting overnight delivery of sample containers will be invoiced for freight. Exygen reserves the right to charge a fee for sample containers. SAMPLE DISPOSAL-- Exygen retains samples for one month after - reporting results, then disposes of or returns the sample. Unless the client requests that the sample(s) be returned, or prior arrangements have been made for long-term storage, Exygen shall dispose o f the sample(s). Exygen shall charge a monthly fee for long-term storage. Samples found or suspected to contain hazardous waste, according to definitions in state and /o r federal guidelines, will be returned to the client upon completion o f the analysis. The cost of returning the sample(s) will be invoiced to the client. Exygen reserves the right to charge a disposal fee for the disposal of any and all samples unless returned by Exygen to client. Exygen shall, unless the nature and character o f the sample dictates otherwise, store all samples under locked, temperature-controlied conditions. An interna! chain-ofcustody is maintained for each lot o f samples received. HAZARD COMMUNICATION--The client has the responsibility to inform the laboratory of any known or suspected hazardous characteristics of the sample, and-to provide information on hazard prevention and personal protection as necessary or otherwise required by applicable law. Q UALITY ASSURANCE--Exygen will perform services consistent with its Quality Assurance Standard Operating Procedures (SOPs), the terms of which are expressly incorporated herein by reference; provided, however, it shall be the exclusive responsibility o f the client to confirm that Exygen's standard practices will meet the client's needs prior to placing an order for work. In the event client desires an alternative to these SOPs, such requests must be made in writing prior to sample submission and acceptance by Exygen. ETHICS POLICY--Exygen Research strives to provide its clients with the highest quality data in the fastest realistic turnaround time. 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These costs shall include, but are not limited to, hourly charges for the persons involved, travel, mileage, and accommoda tions, and for any and all other expenses associated with said litigation, INDEM NIFICATIO N, LIABILITY, A N D INSURANCE-- Exygen agrees to indemnify, defend, and save the client, its officers, directors, employees, agents, and representatives harmless from all losses, expenses, demands, and claims made against the client, its officers, directors, employees, agents and representatives because of any personal injuries, death, or property damage to the extent caused by the negligence or willful misconduct of Exygen, its employees, agents, or representatives in connection with the performance of services under this agreement, except to the extent such losses, expenses, demands, or claims, occur as a result of the negligent or willful acts or omissions of the client, its officers, directors, employees, agents, and representatives; however, such indemnification and damages shall, in the aggregate, be limited to the amount equal to the lesser of (a) damages suffered by the client as the direct result thereof, or (b) the total amount paid to Exygen for the work herein covered, Exygen will, if requested by the client, furnish certificates of insurance from its carrier evidencing appropriate insurance coverage, WARRANTY A N D LIM ITS OF LIABILITY--In accepting analytical work, Exygen guarantees the accuracy of the test results the sample as submitted within the tolerances set forth in the SOPs. We disclaim any other warranties, expressed or implied by law. Exygen does not accept any legal responsibility for the purposes for which client uses the test results, Exygen will not accept any purchase order or any other order for work that includes conditions that vary from these Standard Conditions. ACCEPTANCE OF PURCHASE ORDER--This Purchase Order becomes a binding agreement, subject to the specific terms and conditions stated herein, upon Exygen's commencement of work. 000289 * tj Recovery Summary for PFOA in W ater n tJ PFOA tv f 4;. Sample Amount Amt Found Amount Spiked in Sample Recovered Recovery Description (ng/mL) (ng/mL) (ng/mL) (% ) ^"1 DSN001 ' 500 ng/mL Spike 500 1130 1640 102 N n t{ rj F( i n n u n 000290 n V o s3058 Research Drive State College, PA 16 8 01 , USA f i T: 800.281.3219 V F: 814.272.1019 t exygen.com 3058 Research Drive State College, PA 16801 Phone:814-272-1039 Fax: 814-231-1580 Login#: L0001297 > 1,407 I - , Project: P0000449 ' Project Title/Type: Analysis o f PFO A in W ater / R O U T IN E : Project Storage: Submitted By: Neal Waddell and Randy Roussel Status: Unreceived Login Type: Started: Date Start: Due Date: Received Date: Received By: Immediate Receipt of Samples T 11/12/2003 12:52:36PM 11/26/2003 11/12/2003 ROBB, SHAWN ' Spread Sample: Label: _Login Notes: Conform Notes: Conform COC: Conform Sample: Conform Request: True True True True Package HK0001866 Carton Packages / Containers Mail Date / Condition Shipper /JD Temp. Control / Temperat 11/12/2003 11:15:13AM Package & Contents Uncompromised FEDEX 840238618882 WETICE 1.30 Direction / Handled By RECEIVED ROBB, SHAWN Container # C0015146 Gross Weight fi Container Type 625.7 g 500 ml Clear Plastic Miscellaneous Item Key None Description Preservative NONE ICOC Mfg. Lot 3-140-011 Mfg. ID 559998 Sample ID 10001297-0001 Matrix LIQUID Fraction Water Sample DSN001 Samples .0001297-0001 Container C0015146 / 500 ml Clear Plastic / NONE :-- 11/12/2003 Login.rpt Bottles Method Report Version: Oct 23 2003 9:55AM Page 1 of 1 000291 Instance: R0072518 R0072518 0D292 CHAIN OF CUSTODY/ANALYSIS REQUEST FORM PROJECT IN F O R M A T IO N Exygen Research Sample Receiving *3 1 1 7 Research Drive State College, PA 16801, USA T: 814.231.8032 * F: 814.231.1580 * exygenresearch.com Page / of / ANALYSES REQUESTED C lie n t (nam e & address): c4`/`<A vsie, e,'CO AO. Sox 2 2 -fZ A e c ^ A r, A U ~3 5~6 O ? ___ Phone: 3 <s>6 - jy 'c 'ccs Fax: Z t L - ? o 6 - 5 ~ i 3 z. S a m .p le r: ----- ------------7-&y V--A---^------------------------_-_--_--_-------- P ro je ct M a n a g e r (N am e & E -m ail A ddress): A<a/ J a.gA c& J / A a i/S S a -/ /fotzVToe/<P /)& ; *, fw est'C t >C o r1 P roject N am e: P ro A S T o J*s RO. # : / A 0 3 A Z.2 3 3 o Q u o ta tio n # : Please f ill o u t th is fo rm co m p letely to ensure c o rre c t analysis and p ro p e r h a n d lin g o f y o u r sam ples. O 1- SAMPLES/AZON/ ALYSISClient Sample Identification -Q Collection Collection id l/l OQ. 41.5 .a id E Sc o 3o Date Time u z u Specify Matrix U l'jd . X __pJTpDl * Comments 2 V Ar. L .'ffltA P A -J /A/o-o^ I X LAB USE ONLY CHAIN OF CUSTODY Cooler ID # OTHER INFORMATION l.. I re.A .. Cc>o/c r' LAB USE ONLY ~ o 7T T k / 9 o * T S A A~ L. Cooler Temp. (C) L 3 PROJECT REQUIREMENTS Results Deadline: Laboratory Report Options: CD Sample results only CD Add case narrative CD Add quality control summary CD Add calibration summary CD Add raw data CD Other__________________ L l .. V. 3-4. **b' t ,, ______ ,, - N 5a ExpressPankap/;Service , ; ! | D | g Bn'i8M PackagesuplolXIbs. ' vl f S s S " V /'"i553C i * M.-t . , 1 '!&'.* / | / # :-W ^S sn W s-M - /, " / / .( }, i s / ,.- . M . ..* ( " * y " y ` \>" :^------ i '-*l'.<ii ! * 1' ,*rn i- ' ' 5 A 3 0 6 - S sj'q -`n fa?'- - , ____v ,f,,t I ===! ! ^ ^ a a i ! a ^ ^ '^ - ^ ---- :---------* P te ^ e r n m m X ^ ,, -'viX'-' X 4b ExpfissFr$i|ttSemite ^ , *-j " \ '. i- x ' K., 'Z \ .;U >, _,, _H__ __w_--_ !__-t--_-a-_-_---t_---s". .M ~ t 4 _______ a s t%- ' %] & ' A. ' ,-_*' - f f -* ,- * f- ^ Hta-Mu-.-sl,Nebt|ri*psy. k. .". :X . 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ZIP /( P X L t------:---------- IUI iJS i& X fg. . - ^ 111 t'Y3t1-fr'Viy,?r-*. -JtV ' ' r ( < - " 1 r<nM A o H flM ? jV W t O W wtow " -- rtT-, BEST COPY AVAlLABLt n M Oo o e x - c; c i: e x lx: c . .,. . ' Vm"r'~J-r--i-~iit fL-t^fAT --a., jp' er=-'"k'S-?S---' t|a^^'c5ii".i'*i-" 1 Ik'awas.M'* <' . -.bC' J' %r M % 1j ' . n ft 1[- J, f*"> [` -- t flc i 1 n Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site: NA L1297 PFOA 413 -> 369 NA RAW DATA REPORT Limit of Quantitation: Injection Volume: Matrix: Sample Volume: Final Volume: 50 ng/L 15 pL Water 40.0 mL 5.0 mL Exygen ID XC111003-0 XC111003-1 XC111003-2 XC111003-3 XC111003-4 XC111003-5 XC 111003-6 Methanol Wash 0106020 Control 0106020 Spk A 0106020 Spk B L1297-1 Spk C L1297-1 LI297-1 Rep XC111003-1 XC 111003-2 XC111003-3 XC111003-4 XC111003-5 XC111003-6 Sponsor ID---NA NA NA DSN001 DSN001 DSN001 - Sample Code c CS CS CS CS CS CS c c LCS LCS LF S CsS CS CS CS CS CS Run No. 111703F-901 111703F-902 111703F-903 111703F-904 111703F-905 111703F-906 111703F-907 111703F-908 111703F-909 111703F-910 111703F-911 111703F-912 111703F-913 111703F-914 111703F-915 111703F-916 U1703F-917 111703F-918 111703F-919 111703F-920 PFOA Found (ng/L) = (peak area - intercept) / slope x DF Recovery (%) = [PFOA found (ng/L)-PFOA found in control (ng/L)] amount PFOA added (ng/L) Std. Cone. Dilution (ng/L) Factor 205 -50 - 210500 500 - 10-00 -- 25 1 1 1 2000 2000 20-00 50 - 210500 - 500 - 1000 - x 100 Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: 111703F Karen Risila LC/MS/MS Unit # 7 11/17/03 11/24/03 Peak Area 770 4761 9595 18755 48235 104140 175169 573 368 8949 86532 148346 102360 100355 4652 9230 17675 46474 97299 165644 Amount PFOA PFOA Found Added Recovery (ng/L) (nfi/L) <%) -- -- -- - - - - - -- - -- --- ND 47.0 50 476 500 94 95 1640000 1130000 1100-000 - 500000 -- 10-2 - --* --- Standard Curve : Linear (1/x weighted) Intercept = 454.318 Slope = 180.825 Coef. OfDet = 0.988134 CS = Calibration standard C S ==5SaCmopnlterol sample LF a=Lab fortified sample FF ss Field fortified sample LCS = Laboratory Control Spike CK = Check Standard ND = Not detected = Response between 0 and LOD NQ = Not quantifiable = Response between LOD and LOQ Spreadsheet prepared by: * 000294 j n 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 Internal Chain of Custody/Fortification Sheet Exygen Study Number: L1297 Matrix: Water Sponsor Study/Protocol No: NA The samples listed below were removed from refrigerator No. 3 2 Time lO \S ________ Date l l l n l o s _______ Initials CEE r: 0106020 Control f"! ti 0106020 Spk A 40.0 2.0 0106020 SpkB 40.0 20.0 L1297-1 SpkC 40.0 20000.0 L1297-1 40.0 L1297-1 Rep 40.0 t; I- 1 * All samples were measured: Time |in O ________ Date h |l~ l|o A Initials G c E After measuring samples were returned to refrigerator No. 32 Time 11 S O _________ Date U 'l l ] p 3 Initials C ' Comments: 200 p.L of 250 mg/raL sodium thiosulfate was added to all samples before spiking. Initials/Date: fjSEj/ t f j n j o 3 Analysis Summary: Data Set: u n c s f Data Set: v Data -- Set extraction/analysis data verified by: Initials/Date:. Initials/Date:. Initials/Date: Date:: n te u U > 3 Jkuly/26,*2001/6 000295 3m 1 zzi enPresearch 3058 Research Drive State College, PA 16801 ru Phone: 814-272-1039 Fax: 814-231-1580 i 1 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: L1297 MATRIX: Water METHOD: ANALYTES: PFOA PROTOCOL NUMBER: NA Client ID na na na DSN001 DSN001 DSN001 - Exygen ID 0106020 Control 0106020 Spk A 0106020 Spk B L1297-1 SpkC L1297-1 L1297-1 Rep - STEP STEP 12 1/\ N -- Dilutions (mL-/mL) - 3 At.--0.0A5./o [)-y,o.oA/ . o - STEP 3 \( - Dilutions (mL/mL) - - - - STEP 4 -- - - Reagents/ Materials Methanol C18 SPE Type I Water . - Lot# /J3lbf3U o lAl NA - - - -- - --- - - - - -- - --- - - - - - - - - - - Initials/Date njn(o3. - - -- - --- - . - -- - --- - - _ - -- - - -- - - - - -- - -- - - - - - -- - --- - - - - -- - --- - - - - -- - - -- - - _ - -- - -- _ - -- - -- _ - -- - -- _ - -- - -- _ - *Initials/Date Inba-Car life- -- . -- <Xe- -- - n ]n lo 3 -- SSSSTTTTEEEEPPPP 4231:::: LLFSiPCCnE//aMMlcvoSSol//uMMlummSSneracentlaoaenla5yanls-myiussLpis.collected in 15 mL polypropolene tubes (D bf-IO C D -- - YSWIS*- HPLC - Methanol - Ammonium Acetate - Type I water NA 3- Initials/Date 000296 initials and date under each step indicates the personnel that performed this step. $$ Method of Analysis for the Determination of Perfluorooctane sulfonate (PFOS), Perfluorooctane sulfonylamide (PFOSA), and Perfluorooctanoate (POAA) in Water COMMENTS: Final extracts stored in refrigerator 3 2 - Initials: C&5 Date: li/n /O E July 19, 2001/4 Il T Z ::i :z:i ii 1 i -'J f - 'W' r-fe j , ,^ f - y~| "3 g l:en RESEARC H 3058 Research Drive State College, PA 16801 I Phone: 814-272-1039 Fax: 814-231- >gen STUDY N O . u x a PREPARATION OF EXTRACTED CALIBRATION STANDARDS Protocol No.: None Method No.: 01M-008-046* Exygen Study No.: NA Analytes: PFOA Matrix: Type I WaterA Sample Vol: 40 mL Sponsor Sample ID NA NA NA NA NA NA NA Exygen Sample ID 0106020 0106020 0106020 0106020 0106020 0106020 0106020 Sample Description Type I WaterA _Fort. Solution Fort. Fort. Micropipet Soin. Cone. Volume used Fort. Level ID (ML) fuL) (DPt) Final Solution ID #** _ - - XC111003-0 Type I WaterA F092203-5 10 100 200 25 XC111003-1 Type I WaterA F092203-5 10 200 200 50 XC111003-2 Type I WaterA F092203-5 10 400 200 100 XC111003-3 Type I WaterA F092203-4 100 100 200 250 XC111003-4 Type I WaterA F092203-4 100 200 200 500 XC111003-5 Type I WaterA F092203-4 100 400 200 1000 XC111003-6 Reagents/ Materials Lot# Methanol 4 3 m 3 3 S C18 SPE U 3 2 0 H B I Type I Water NA -- -- -- -- NA 0106020 Type I WaterA F102703-2 Vertical arrows in a-column indicate identical values. - 100 - 100 - 200 - 250 - X C 1 11003-7 - Initials/Date: ){\iO [o **This must be a unique number. Use this system: Extracted Calibration Soln ID #: Samples removed from ^fngeratOr^freezer # 37~___ Time: .CfiCO.. 40 mL of each sample measured using a S O mL graduated cylinder. After measuring, samples returned to (^ffigaramrAfreezer # 3 3 r . Time:/2SL XCMIMniDtiaDlsY/DY-a0t,e1:,2i,E'3.EeLtc. Initials/Date: A S T Tnitials/Date: 2 F ! hjtojn? / lljiajt. / iljtojo? H A-c-XAC i"GC-A / G.; ORIGINAL D O CU M EN T B A T E - l^ lS - Samples fortified: Initials/Date:. T2|7 / n [\i)'o 3 SPE clean-up: Initials/Date:. Final volume adjusted to 5 mL: Extracts placed in refrigerator # S 2 - Initials/Date: CkB-.. Initials/Date: (._ / u L ' , Ins. STANDARD EXPIRATION DATE: 11/24/03 Comments: AThis type I water has been filtered through a hypercarb filter * Method of Analysis for the Determination of Ammonium Perfluorooctanoate (APFO) in Water. <ro0 July 10,2001/0 ! Masslynx - Sample List Sample List: C:\MASSLYNX\008 APFC t.PRO\SampleDB\111703F.spl Printed: Mon Nov 24 11:22:23 2003 l f r u b t l o B ______________ Vial File Name LIMS ID Client ID Sample Description 1 1 111703F-901 -- 2 2 111703F-902 -- 3 3 111703F-903 -- 4 4 111703F-904 -- 5 5 111703F-905 -- 6 6 111703F-906 -- 7 7 111703F-907 -- 8 92 111703F-908 -- 9 31 111703F-909 -- 10 32 111703F-910 -- 11 33 111703F-911 -- 12 34 111703F-912 -- 13 35 111703F-913 -- 14 36 111703F-914 -- 15 2 111703F-915 -- 16 3 111703F-916 -- 17 4 111703F-917 -- 18 5 111703F-918 19 6 111703F-919 -- 20 7 111703F-920 -- XC111003-0, 0 ng/L standard XC111003-1, 25 ng/L standard XC111003-2, 50 ng/L standard XC111003-3,100 ng/L standard XC111003-4, 250 ng/L standard XC111003-5, ,500 ng/L standard XC111003-6,1000 ng/L standard Methanol Wash 0106020 Control 0106020 Spk A, 50 ng/L 0106020 Spk B, 500 ng/L L1297-1 Spk C, 500000 ng/L, DFL1297-1, DF=2000 L1297-1 Rep, DF=2000 XC111003-1, 25 ng/L standard XC111003-2, 50 ng/L standard XC111003-3,100 ng/L standard XC111003-4, 250 ng/L standard XC111003-5,500 ng/L standard XC111003-6,1000 ng/L standard Exygen STUDY NO Page 1 Page Position: (1,1) Matrix Sample Type Cone (ng/L) Cone B Cone C Test ID DF MS Method -- -- =2000 -- -- -- -- Blank Standard Standard Standard Standard Standard Standard Blank Blank QC QC QC Analyte Analyte Standard Standard Standard Standard Standard Standard 0 25 50 100 250 500 1000 50 500 500000 25 50 100 250 500 1000 -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- . . . 0 1 008 PFOA -- 0 1 008 PFOA -- 0 1 008 PFOA -- 0 1 008 PFOA -- 0 1 008 PFOA -- 0 1 008 PFOA -- 0 1 008 PFOA -- 0 1 008 PFOA -- 0 1 008 PFOA -- 0 1 008 PFOA -- 0 1 008 PFOA -- 0 2000 008 PFOA -- 0 2000 008 PFOA: -- 0 2000 008 PFOA: -- 0 1 008 PFOA -- 0 1 008 PFOA -- 0 1 008 PFOA -- 0 1 008 PFOA -- 0 1 008 PFOA -- 0 1 008 PFOA Masslynx - Sample List Sample List: C:\MASSLYNX\008 APFO. PRO\SampleDB\111703F.spl Printed: Mon Nov 24 11:22:23 2003 Hb{?03 HPLC Method MS Tune File Inj Volume (pL) 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 water water water water water water water water water water water water water water water water water water water water PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOA Tune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune 1111111111111111111155555555555555555555 Exygen STUDY N O . f c ! l Page 2 Page Position: (2,1) LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exygen Study No: L I297 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #7) Computer: COMPAQ Professional Workstation AP200 Software: MMiiccrroomsoafstsWLiinmdiotewds: NMTa:sVsLerysnioxn34.4BBuuiilldd 1030841: Service Pack 5 HPLC Equipment: HewHHlPPetAQt PuuataoctskPaaumrmdppl(eHrP) Series 1100HHPP CVoalcuumumn ODveegnasser HPLC Column: G(JeOnNesEisSCCH-8R, 5OcMmAxT2O.1GmRAmPiH.dY. x: P4aprt(NExoy. gFeKn5I9D6:2MEAJ)10464) MMoobbiillee PPhhaassee ((AB)) :: 2MmetMhanAoml monium Acetate in Type I Water Analyst: EPK30hxa5oyr8negneeR:nRe(Ri8sse1eha4sare)cah2r7cDh2r-i1v0e3,9StFatAeXC:o(ll8e1g4e), 2P3A1-115688001 (j NOTE: Ttinhhseetrmnueamxssteln3ytnpsxaegtsteoisfntagwrsaeurcesoepdmrfopogurrtaethrmeg.aenTneahrleyaspteiasdgoepfsrtichnoitsnotduaatistnaftrshoeemt. All Handwritten Peak ID 's by:_____ Z __________ 000300 n Scanning Method Report I" 4. Method: Last Modified: C:\MASSLYNX\008 APFO.PRO\ACQUDB\008 PFOA Wed Mar 20 15:07:50 2002 I- : Printed: Mon Nov 24 11:22:41 2003 n |2 M o 3 " Solvent Delay ( mins ) : 0.00 Function : 1 t: MRM of 1 Mass Pair ( ESP- ) k"' Inter Channel Delay ( Secs ) : 0.03 Span ( Daltons ) : Start Time ( Mins ) : , End Time ( Mins ) : 008 ... 000 000 Repeats : 1 Channel Parent Daughter Dwell (Secs) Coll Energy (eV) ft.^ r * 1 413.00 369.00 0.20 10 Cone ( V ) 10 Page 1 .31 I' if fe. i w tke- yi! 000301 Method Report Method File: Last Modified: Printed: C :\MASSLYNX\08 PFO.PRO\ACQUDB\water Monday, November 24, 2003 11:19:02 Monday, November 24, 2003 11:22:48 HP1100 LC Pump Initial Conditions Solvents A% B% C% D% SO.O 40.0 0.0 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 0.300 15.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 10 entries which are Time (jSran*rj; 0.00 0.40 1.00 7.00 7.50 9.00 9.50 13.50 14.00 ^ 15.00 A% 60.0 60.0 10.0 10.0 0.0 0.0 60.0 60.0 60.0 60.0 B% 40.0 40.0 90.0 90.0 100.0 100.0 40.0 40.0 40.0 40.0 C% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0,0 0.0 . 0.0 HP1100 LC Pump External Event Timetable The Timetable contains 4 entries which are : <j Time Column Switch Contactl Contact2 !, Initial 0.00 Off Off Off Off On Off f ; 0.10 Off Off On 8.00 Off Off Off Sr" HP1100 Autosampler Initial Conditions Draw Speed f } Eject Speed (/nl/min) V ' Draw Position (mm) *.' Stop Time (mins) Injection Volume (/il) p-a Vial Number 200.0 200 0.10 15.00 15.0 1 D% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 Contact3 Off Off Off Off Flow 0.300 0.3 00 0.300 0.300 0.300 0.400 0.400 0.400 0.300 0.300 Contact4 Off Off Off Off Page 1 Pressure 400 400 400 400 400 400 400 400 400 400 n I4 000302 Tuning Method Report Method: C:\MASSLYNX\008 A P F O .PRO\ACQUDB\PFOA TUNE Printed: Mon Nov 24 11:22:57 2003 Page 1 SOURCE ( ESP- ) Capillary Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp. Set Rdbk 3.00 10 0.0 0.0 0.0 100 300 -2.93 -10 101 300 Pressures Analyser Vacuum Gas Cell Rdbk OFF 3. le-3 Analyser LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas Flows Cone Gas Desolvation Set Rdbk 14.0 14.0 1.0 -2 10 2 14.0 14.0 2.0 700 8 9 11 -695 Rdbk 79.0 707.3 000303 t Quantify Calibration Report L. Study No.:L1297, Set N o . :111703F, Ext.Date:ll/17/03, Analyst:K.Risha Page 1 Exygen Research, 3058 Research Drive, State College, PA 16801 000304 Quantify Sample Report Study No.:L1297, Set No.:111703F, Ext.Date:ll/17/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111703F ii\ Last modified: Tue Nov 25 07:25:32 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 . r * Job Code: Printed: Tue Nov 25 07:28:29 2003 Initials Date__ { aJSlQ, Run# ja i I' i Name: 111703F-901 Text : Page 1 f. < *** -n( * t Ij ti Exygen Research, 3058 Research Drive, State College, PA 16801 000305 H I: I ; Quantify Sample Report r! Study No.:Ll297, Set No.:111703F, Ext.Date:ll/17/03, Analyst:K.Risha I*; Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111703F ` i Last modified: Tue Nov 25 07:25:32 2003 1 ' Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Tue Nov 25 07:28:29 2003 fS Name: 111703F-902 Text: 1: PFOA Page 2 fS'-*V ( ki r* l\ - r* I ( . '' " &fr ; ... Exygen Research, 3058 Research Drive, State College, PA 16801 n .... ? 000306 Quantify Sample Report Study No.:L1297, Set N o . :111703F, Ext.Date:ll/17/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111703F Last modified: Tue Nov 25 07:25:32 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Tue Nov 25 07:28:29 2003 Name: 111703F-903 Text: 1 : PFOA Page 3 Exygen Research, 3058 Research Drive, State College, PA 16801 000307 n &i f Quantify Sample Report Study No.:L1297, Set No.:111703F, Ext.Date:11/17/03, Analyst:K.Risha t * . Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111703F I i Last modified: Tue Nov 25 07:25:32 2003 * Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 r Job Code: Page 4 Printed: Tue Nov 25 07:28:29 2003 fn l ; Name: 111703F-904 Text : f- , 1: PFOA .. XC111003-3,100 ng/L standard i 111703F-904 Sm (Mn, 2x2) 100- - i * %- , . 5.44 18755 24-Nov-2003 13:59:41 LC/MS/MS #7 M RM of 1 Channel ES413 >369 3.96e5 Area 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 * o: i-'i ri-riilTs1`lrp1i1i1i1iIi""fi"""'i1 1i1irr-rr"i' Tt '''iP--i--" 'i-r' 'r"Ii"iiIii iI r1 i1 i1 i1 iI i1"i1 i1 i1 Ii1i1t n1 1 I|h1 1t1'1 I 1iT1r1~r,.ff rrrrI,'i<,--Tr--,I II Ii rr-Ii'!iI|IiIi-triI I|TI im e p- >< t I .r ! i. i is 1i n Exygen Research, 3058 Research Drive, State College, PA 16801 000308 rn t! n K - Quantify Sample Report Study No.:L1297, Set No.:111703F, Ext.Date:11/17/03, AnalysttK.Risha i kI Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111703F Last modified: Tue Nov 25 07:25:32 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Tue Nov 25 07:28:29 2003 Name: 111703F-905 Text: "S Page 5 M f* : >1 U--' p a', if t f 4 _ Exygen Research, 3058 Research Drive, State College, PA 16801 n\ \ - : = *-. - ^ .............. . 000309 n | i Quantify Sample Report Study No.:L1297, Set No.:111703F, Ext.Date:ll/17/03, Analyst:K.Risha f"! Sample List: P:\Data\LCMSMS7\MasslynK\008 APFO.PRO\SampleDB\111703F i Last modified: Tue Nov 25 07:25:32 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 fft"! Job Code: * Printed: Tue Nov 25 07:28:29 2003 Page 6 Name: 111703F-906 Text: 1 : PFOA XC111003-5, 500 ng/L standard t ' 111703F-906 Sm (Mn, 2x2) 100i r*i fc \ %: 5.43 104140 24-NOV-2003 14:33:24 L C /M S /M S # 7 MRM of 1 Channel ES413 >369 2.09e6 Area 1.00 2.00H 0-J '" T"T l T l l-T'l | I I I -I- | ! T-l I pi i i i r i i p-r-i i-T- 1 i--r""i i--pr < 1 i | I- 1 i i i i i i i i t I | vi it r *1I I I I1-I I v r-| Time 3.00 4.00 5.00 6.00 7.00 8.00 h*. r '< I ' n 13 I- ' pm, I* I* n Exygen Research, 3058 Research Drive, State College, PA 16801 n 000310 n .p i Quantify Sample Report Study No.:L1297, Set No.:111703F, Ext.Date:ll/17/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111703F Last modified: Tue Nov 25 07:25:32 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Tue Nov 25 07:28:29 2003 + i Name: 111703F-907 ` Text : Page 7 n *' i n f- i Exygen Research, 3058 Research Drive, State College, PA 16801 m t. 00031 Quantify Sample Report Study No.:L1297, Set No.:111703F, Ext.Date:11/17/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111703F Last modified: Tue Nov 25 07:25:32 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Tue Nov 25 07:28:29 2003 Name: 111703F-908 Text: 1: PFOA Page 8 Exygen Research, 3058 Research Drive, State College, PA 16801 000312 Quantify Sample Report Study No.:L1297, Set No.:111703F, Ext.Datesll/17/03, AnalysttK.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111703F Last modified: Tue Nov 25 07:25:32 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Tue Nov 25 07:28:29 2003 Name: 111703F-909 Text: 1: PFOA Page 9 Exygen Research, 3058 Research Drive, State College, PA 16801 000313 Quantify Sample Report Study No.:L1297, Set No.:111703F, Ext.Date:ll/17/03, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111703F , Last modified: Tue Nov 25 07:25:32 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: Printed: Tue Nov 25 07:28:29 2003 Name: 111703F-910 Text : 1: PFOA Rage 10 Exygen Research, 3058 Research Drive, State College, PA 16801 000314 n l ' Quantify Sample Report ; Study No.:L1297, Set N o . :111703F, Ext.Date:11/17/03, Analyst:K.Risha r-< i Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111703F Last modified: Tue Nov 25 07:25:32 2003 - Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 f~ i Job Code: Printed: Tue Nov 25 07:28:29 2003 i Name: 111703F-911 1 Text : Page 11 f; ri I^ t1 H ! ' Exygen Research, 3058 Research Drive, State College, PA 16801 m 000315 r"5 ............. , Quantify Sample Report 1 I; Study No.:L1297, Set No.:111703F, Ext.Date:11/17/03, Analyst:K.Risha Page 12 ft Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111703F ; Last modified: Tue Nov 25 07:25:32 2003 - Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 f"i Job Code: t j- - - ' "' Printed: Tue Nov 25 07:28:29 2003 n ? Name: 111703F-912 Text: 1: PFOA L1297-1 Spk C, 500000 ng/L, DF=2000 111703F-912 Sm (Mn, 2x2) *t - ! 100n fe. J %: 5.46 148346 24-NOV-2003 16:14:42 LC/MS/MS #7 M RM of 1 Channel E S 413 > 3 6 9 1 ,9 6 e 6 Area O ' ' I I T- r I" i-j - f I i I I 1I I i t I I ! i I | i i 1- r I I t 1.00 2.00 3.00 4.00 5.00 6.00 r i i" ''" 1' 1 1 t t t t ] - i 't-t-i 'i T im e 7.00 8.00 f- ! f"- t n r Ii $u j ! * n Exygen Research, 3058 Research Drive, State College, PA 16801 n ?; 000316 n f i .. .. I ; Quantify Sample Report - Study No.:L1297, Set No.:111703F, Ext.Date:11/17/03, Analyst:K.Risha ' Page 13 r~ Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111703F !"` Last modified: Tue Nov 25 07:25:32 2003 i Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 l~ ': Job Code : Printed: Tue Nov 25 07:28:29 2003 r~ t k Name: 111703F-913 Text: f"! 1 : PFOA L1297-1, DF=2000 1 1 1 7 0 3 F -9 1 3 S m (Mn, 2 x 2 ) 1OOn t %: 5 45 102360 24-NOV-2003 16:31:33 LC /M S/M S #7 MRM of 1 Channel ES- 413 >369 1.36e6 Area r-- n i n *I t 0 ' ' I I ' > r r | -I I ' I I I V", r | - " r 1.00 2.00 3.00 TT 4.00 5 .0 0 6.00 i " r " 1 i 1 1 '.' I Tim e 7.00 8.00 ( i Exygen Research, 3058 Research Drive, State College, PA 16801 R 000317 m Ir ; L ' Quantify Sample Report Study No.:L1297, Set No.:111703F, Ext.Date:11/17/03, Analyst:K.Risha Page 14 Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111703F Last modified: Tue Nov 25 07:25:32 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 Job Code: i: \ Printed: Tue Nov 25 07:28:29 2003 n Name: 111703F-914 Text: 1 : PFOA U 297-1 Rep, DF=2000 1 1 1703F-914 Sm (Mn, 2x2) 10CH r *i s AK 100355 24-Nov-2003 16:48:20 LC/MS/MS #7 M RM of 1 Channel ES413 >369 1 .34e6 Area 1.00 T ' 111' ' 2.00 3.00 -pr-r-r-r-pr-r 4.00 5.00 6.00 i I I i I I I I Time 7.00 8.00 tr * !j i M . i t n (? ? n Exygen Research, 3058 Research Drive, State College, PA 16801 000318 | Quantify Sample Report Study No.:L1297, Set No.:111703F, Ext.Date:11/17/03, Analyst:K.Risha r-> Sample List: P:\Data\LCMSMS7\Masslynx\008APFO.PRO\SampleDB\111703F ; : Last modified: Tue Nov 25 07:25:32 2003 L Method: P:\Data\LCMSMS7\Masslynx\008APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 jPt ; Job Code: - f' Printed: Tue Nov 25 07:28:29 2003 I Name: 111703F-915 Text : Page 15 if-- H 0 n 'ik- . L. n Exygen Research, 3058 Research Drive, State College, PA 16801 p ..... ..... ........ 000319 t i Quantify Sample Report 1 Study No.:L1297, Set No.:111703P, Ext.Date:ll/17/03, Analyst:K.Risha Page 16 r* Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111703F i j Last modified: Tue Nov 25 07:25:32 2003 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 f 1 Job Code: Printed: Tue Nov 25 07:28:29 2003 n ,: . f Name: 111703F-916 Text: .... , ......... ' :: -: ~ ---------------- ; ~ H 1 : PFOA__________________________________________________________________________________________________________________ |XC111003-2,50 ng/L standard f :r i 1 1 1 7 0 3 F -9 1 6 Sm (M n, 2x2) 100n it. ;! % : 5.46 9230 24-Nov-2003 17:21:57 LC/MS/MS #7 M RM of 1 Channel ES413 > 3 6 9 1.86e5 Area ni V 0: n .n"|'i'.|rT ,')',"rrTT ) i t'T \ j i r i i \ .j--i-t t -t i-t i t i | i v i i j i'Tm,i *i vt -i i i i - i "i~i~i ) r-~rt i--n i"ir;"i-i i i-| T im e 1.00 2 .0 0 3.00 4 .0 0 5.00 6.00 7.00 8.00 f t fi. r** * .{ t n (T3 fi. i * Exygen Research, 3058 Research Drive, State College, PA 16801 000320 tn ( i Hi Quanti. fy Sample Report ' Study No.:L1297, Set No.:111703F, Ext.Date:ll/17/03, Analyst:K.Risha r- Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111703F f : Last modified: Tue Nov 25 07:25:32 2003 ' Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 PI Job Code: Printed: Tue Nov 25 07:28:29 2003 Name: 111703F-917 Text: Pag'e 17 n I; H n M 1i n fi Exygen Research, 3058 Research Drive, State College, PA 16801 P ' ' ' l> 000321 I r-f -, : .......................... f ? Quantify Sample Report " - : ; Study No.:L1297, Set No.:111703F, Ext.Date:ll/17/03, Analyst:K.Risha r*> Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111703F l Last modified: Tue Nov 25 07:25:32 2003 ' Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 k \ Job Code : M Printed; -- Tue Nov 25 07:28;29 2003 n f ' Name: 111703F-918 Text: Page 18 n fI*--; n f! I n r f t i Exygen Research/ 3058 Research Drive, State College, PA 16801 000322 jT"3 rj I j Quantify Sample Report i Study No.:L1297, Set No.:111703F, Ext.Date:ll/17/03, AnalystsK.Risha f - l Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111703F I j Last modified: Tue Nov 25 07:25:32 2003 : Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 jp* Job Code: " Printed: Tue Nov 25 07:28:29 2003 Name: 111703F-919 Text : 1: PFOA f' n jf. !, t'.j fi r-> Page 19 Exygen Research, 3058 Research Drive, State College, PA 16801 000323 n | i . - Quantify Sample Report . - " Study No.;L1297, Set No.:111703Ff Ext.Date:11/17/03, AnalystsK.Risha f" Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111703F t 1 Last modified: Tue Nov 25 07:25:32 2003 1 ' Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\111203 PFOA Last modified: Fri Nov 14 10:37:34 2003 P Job Code: ll - ' '' Printed: Tue Nov 25 07:28:29 2003 Page 20 I ] Name: 111703F-920 Text: 1 : PFOA XCt 11003-6,1000 ng/L standard 111703F-920 Sm (Mn, 2x2) L j 100- %- 5.48 165644 24-Nov-2003 18:29:24 LC/MS/MS #7 M RM of 1 Channel ES413 > 3 69 3.14e6 Area 0 : ... ' T 1 , ~r '`1 1I T1 1' "1 ' 1I "1 1 11 11 1I 11 ' 11 1 I ' 1.11 1l~rI ~l1...1..1. 11 1I 11 11 l1~ T1~ "lI ''1 11 11 11 1I 1 1111 1 I 1 1 1 1 I 1 1 1 1..I...'...1..'' 1I I l'" 1...' ..'.....1..1..T,~ Ir T ! I'' T1 i' m' 1e I 1.00________ 2 W ________ 3XI0________4^00________ 5 .0 0 6 .0 0 7.00 8.00 I: tj F p ti. Exygen Research, 3058 Research Drive, State College, PA 16801 000324