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n L4 t: n t> ; f? i I -I n i. i n n -j l: rh n p"*, R Xth ' P i' fi !" Proven Results. A R A k _ / 7 // Analytical Report Fluorochemical Characterization of Water and Sludge Samples Daikin America, Inc. Exygen Research Laboratory Report No. L0001445 Testing Laboratory Exygen Research 3058 Research Drive State College, PA 16801 Requester Neal Waddell Daikin America, Inc. 905 State Docks Road (35601) PO Box 2252 Decatur, AL 35609 (256) 306-5000 RECEIVED CC-CT">3 TP33OJ CO^23 PO --ipn :i r < zx Li m OO --J PAGE 1 0 F 4 000325 J ^ 3 0 5 8 Research Drive ^ r m s t a t e College, PA 16801, USA 800.281.3219 m F : 814.272.1019 exygen.com )- \ .J ! !( i k*n.*4 fn '> j 'i j ] %i i I n '} ` -'- l ! 1 Introduction ' Results are reported for the analysis of water and sludge samples received by Centre Analytical Laboratories, Inc. (dba Exygen Research) (Exygen) from Daikln America, Inc. This report presents results assigned to Exygen Research study number L0001445. Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC/M S/MS) was requested for all samples. A total of three water samples and one sludge sample w ere received for analysis. The samples were prepared and analyzed by LC/M S/M S for the following list of fluorochemicals: Table 1: T arget Analysis Compound Name Perfluoroctanoic Acid Acronym PFOA 2 Sample Receipt T he samples were submitted in individual plastic containers, cooled with wet ice. Samples were collected on 12/9/03 and 12/11/03 and were received on 12/12/03. 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 40 days of collection. 4 Methods - Analytical and Preparatory 4.1 LC/MS/MS 4.1.1 Sample Preparation for LC/MS/MS Analysis (water samples) Water samples were initially treated with 200 uL of 2 50 mg/L sodium thiosulfate solution to remove residual chlorine. Solid phase extraction (SPE) was used to prepare the samples for LC/MS/M S analysis. A forty-milliliter portion of sample was transferred to a C i8 SPE cartridge. The cartridge was eluted with 40% methanol: water. The eluate was discarded. The cartridge was then eluted with 100% methanol. A 5 mL portion of methanol was collected for analysis by LC/MS/MS. This treatment resulted In an eight-fold concentration of the samples prior to analysis. PAGE2 OF 4 000326 4.1.2 Sample Preparation for LC/MS/MS Analysis (sludge samples) Five grams of sludge were extracted into five milliliters of methanol. The methanol was then diluted to forty milliliters with deionized water. The diluted extracts were submitted to the same SPE cleanup used for water samples. 4.1.3 Sample Analysis by LC/MS/MS A Hewlett-Packard H P1100 HPLC system coupled to a Micromass Ultima M S/M S was used to analyze the sample extracts. Analysis was performed using selected reaction monitoring (SRM). Samples were extracted and analyzed between 12/30/03 and 1/16/04. Exact dates for extraction and analysis are given with the raw data files in Attachment D. 5 Analysis " .;/:V v 5.1 Calibration A 6-point calibration curve was analyzed at the beginning of the analytical sequence and throughout the run for the compounds of interest. The calibration points were prepared at 25, 50, 100, 250, 500, and 1000 ng/L (ppt), as perfluorooctanoic acid (PFOA). The instrument response versus the concentration was plotted for each point. Using linear regression with 1/x weighting, the slope, y-intercept and correlation coefficient (r) and coefficient of determination (r2) were determined. A calibration curve is acceptable if r > 0 .9 9 2 (r2 > 0.985). Calibration standards for M S/M S analysis were prepared using the same SPE procedure used for samples. For the results reported here, calibration criteria were met. 5.2 5.3 5.4 5.5 Blanks Extraction blanks were prepared and analyzed with every extraction batch of samples. Th extraction blanks should not have any target analytes present at or above the concentration of the low-level calibration standard. For these samples, the extraction blanks were compliant. instrument blanks in the form of clean methanol solvent were also analyzed after every highlevel calibration standard, and after known high-level samples. Again, the blanks should not have any target analytes present at or above the low-level calibration standard. For the samples presented here the instrument blanks are compliant. Surrogates Surrogate spikes are not a component of the LC/M S/M S analytical method. Matrix Spikes Matrix spikes were prepared for samples DAI-121003-N W -02 and DA I-092503-N W -02 at levels approximating the sample concentrations. The matrix spike recoveries were within the acceptable range of 70 - 1 3 0 % . Matrix spike recoveries are given in Attachment B. Duplicates Samples DAI-12 1 003-N W -02 and DAI-092503-NW -02 were analyzed in duplicate. Results are given along with the sample results in Attachment A. PAGE 3 OF4 000327 Laboratory Control Samples Miiliq water was spiked with PFOA at 50 and 500 ng/L. with each extraction set. All laboratory control samples showed recoveries between 70 and 130% . Data Summary -=:. .--V X Vvv' ' ' Please see Attachment A for a detailed listing of the analytical results. W ater sample results are reported in (ng/mL) parts per billion as PFOA. Sludge sample results are reported in units of ug/g (parts per million) on a dry-weight basis. Data/Sample Retention Samples are disposed of one month after the report is issued unless otherwise specified. All electronic data is archived on retrievable media and hard copy reports are stored in data folders maintained by Exygen. Attachments Attachment A: Results Attachment B: Matrix Spike Recoveries Attachment C: Chain of Custody Attachment D: LC/M S/M S R aw Analytical Data Signatures : : ^ - ^ " - ''-'. Paul Connolly, T eam Leader-LCMS Other Lab Members Contributing to Data Karen Smith Date Date PAGE4 OF4 000328 r**. " 1 n Proven Results. ri^ r f' Summary of PFOA in Sludge and Water Samples t' Sam ple ID Analyte Found (pg/g) PFOAA n DAI-121003-N W -02 . DAI-121003-N W -02* 29.1 2 8 .3 -t > Analyte Found (ng/mL) C , Sample ID PFOA DAI-121003-NW -01 67.4 DAi-12 1 003-NW -01 * 63.4 DAI-12 1 003-N W -03 599 DAI-12 1 003-N W -FB 0.282 nI*- i. - ` Laboratory Duplicate ADry-weight basis \ C! l ft LJ 0 0 0 3 2 9 m x 3058 Research Drive V>#mstSattate College, PA 16801, USA J: 814.272.1039 F: 814.231.1580 exygen.com STANDARD TERM S A N D CO ND ITIO N S -Services provided by Exygen Research are lim ited to the terms and conditions stated herein, unless otherwise agreed to in a form al contract. CONFIDENTIALITY-- Exygen Research ("Exygen," "us," or "w e") maintains the strictest confidentiality in all of our client interactions, (f a signed confidentiality agreement is required, we will provide one. if a regulatory or Segal body subpoenas information, the client will be notified promptly. The client agrees not to use Exygen's name and/or data in any manner that might cause harm to Exygen's reputation or business. Approval must be obtained, in writing, before Exygen's name can be published in any way. CONTRACTS--All contracts are subject to review and approval by Exygen's legal council and must be signed by a corporate officer. PAYMENT TERMS-- Unless otherwise set forth in this Purchase Order, terms of payment are "Net 30 Days." The time allowable for payment shall begin after both: (a) client's receipt of Exygen's invoice: and (b) the satisfactory performance o f the services contemplated hereunder. A 1.5% monthly service charge shall be added to all past due balances. Notwithstanding any payment terms to the contrary set forth in this Purchase Order, Exygen, in its sole discretion, reserves the right to request payment in advance from client. In the event of default in payment for services rendered, Exygen shall be entitled to reasonable costs of collection, including, but not limited to, attorneys' fees. BILLING--All fees and charges are billed directly to the client requesting services. Exygen will not bill a third party without prior notification in writing, via a signed statement acknowledging and accepting responsibility for payment. Exygen will assume that the paperwork submitted with a sample describes the desired testing protocol. Any changes to the protocol must be submitted in writing. Please fax changes to Exygen marked, "URGENT" to your assigned representative. If changes are made after the originally requested testing has been initiated or completed, the client accepts responsibility for payment. Exygen will not be responsible for hold times that are missed due to such changes. RUSH SERVICE--Exygen routinely offers expedited turnaround times on critical analyses. Rush analysis services are contingent upon availability and prearrangement with an authorized Exygen representative. A surcharge is usually added to the list fee if rush analysis is requested. M IN IM U M FEE--The minimum fee for commercial services is one hundred dollars ($100). SAMPLE COLLECTION/SUBMISSION-- Client shall be responsible for proper collection, preservation, packing and packaging, and shipment of the sample(s) in accordance with applicable law and good commercial, practice. Title and risk of loss with respect to submitted jamles shall at all times remain with client prior to acceptance by an Exygen sample custodian. Exygen will initiate a chain-of-custody upon sample receipt unless the client includes one with the sampler's). By request, Exygen will provide chain-of-custody forms for client's use. All samples submitted must be accompanied by: purchase order, or signed quotation; sample description, including sample type, source, lime and date of collection; specific analyses requested; estimated concentration levels; requested report date; current billing address; and other relevant information. Upon request, Exygen will provide and ship appropriate sample containers to clients. These containers will include the appropriate preservative if particular analyses require one. It is the responsibility of the client to handle these preserved containers safely, and using all appropriate safety precautions. Clients requesting overnight delivery of sample containers will be invoiced for freight. Exygen reserves the right to charge a fee for sample containers. SAMPLE DISPOSAL-- Exygen retains samples for one month after reporting results, then disposes of or returns the sample. Unless the client r requests that the sample(s) be returned, or prior arrangements have been made for long-term storage, Exygen shall dispose of the sample(s). Exygen shall charge a monthly fee for long-term storage. Samples found or suspected to contain hazardous waste, according to definitions in state and /o r federal guidelines, will be returned to the client upon completion of the analysis. The cost o f returning the samplefs) will be invoiced to the client Exygen reserves the right to charge a disposal fee for the disposal of any and all samples unless returned by Exygen to client. Exygen shall, unless the nature and character of the sample dictates otherwise, store all samples under locked, temperature-controlled conditions. An internal chain-ofcustody is maintained for each lot o f samples received. HAZARD COMMUNICATION--The client has the responsibility to inform the laboratory of any known or suspected hazardous characteristics of the sample, and to provide information on hazard prevention and personal protection as necessary or otherwise required by applicable law. QUALITY ASSURANCE--Exygen will perform services consistent with its Quality Assurance Standard Operating Procedures (SOPs), the terms of which are expressly incorporated herein by reference; provided, however, it shall be the exclusive responsibility of the client to confirm that Exygen's standard practices will meet the client's needs prior to placing an order for work. In the event client desires an alternative to these SOPs, such requests must be made in writing prior to sample submission and acceptance by Exygen. ETHICS POLICY-- Exygen Research strives to provide its clients with the highest quality data in the fastest realistic turnaround time. We balance the high standards of this goal by insisting that each employee also perform within the guidelines o f the highest possible professional ethics. Each Exygen employee is required to sign a statement of personal and professional integrity. SPECIAL REPORTS--Additional charges may be necessary for custom report formats. LITIGATION--All costs associated with compliance to any subpoena for documents, for testimony in a court of law, or for any other purpose relating to work performed by Exygen Research shall be invoiced by Exygen and paid by client These costs shall include, but are not limited to, hourly charges for the persons involved, travel, mileage, and accommoda tions, and for any and all other expenses associated with said litigation, INDEMNIFICATION, LIABILITY, AN D INSURANCE--Eo/gen 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 -esult of the negligent or willful acts or omissions of the client, its officers, directors, employees, agents, and representativos; 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 AND LIMITS OF LIABILITY-- In accepting analytical work, Exygen guarantees the accuracy of the test resuits for the sample as submitted within the tolerances set forth in the SOPs, We disclaim any other warranties, expressed or implied by law, Exygen does not accept any legal responsibility for the purposes for which client uses the test results. Exygen will not accept any purchase order or any other order for work that includes conditions that vary from these Standard Conditions. ACCEPTANCE 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. jqh U a a ij a /-i :j a a 3 hi a a a a n 000330 H fl fl f. i t n .J' 4i p. * ; #i n i) n tj n t **& ;' Lj I- i f i' * :4 - Proven Results. Recovery Summary for PFOA in Sludge and Water Sample Description D A I-12 1 003-N W -02 500 ng/mL Spike DAI-92503-NW-02 500 ng/mL Spike Amount Spiked (ng/mL) PFOA Amt Found Amount in Sample Recovered Recovery (ng/mL) (ng/mL) (%) 2500 1780 4340 102 500 67.4 609 108 000331 J K 3058 Research Drive VState College, PA 16801, USA T: 800.281.3219 F: 814.272.1019 exygen.com 3058 Research Drive State College, PA 16801 Project: P0000449 Project Storage: Company Name: Daikin America Submitted By Neal Waddell and Randy Roussel Status: Unreceived Login Type: Immediate Receipt of Samples Started: T D ate Start: t Due Date: 12/12/2003 12/26/2003 Received Date: 12/12/2003 Received By: AMMERMAN, MARK ^ Spread Sample: 1 Label: Project Title/Type: Analysis of P F O A in W ater / R O U T IN E ^ Exygen SD /PI: RISHA, KAREN f- Login Notes: Conform Notes: Conform COC: Conform Sample: Conform Request: True True True n . Package ^JgK0002036 tI Carton Packages / Containers Mail Pate / Condition Shipper/_ID 12/12/2003 10:46:32PM FEDEX Package & Contents Uncompromised3168014911000003840238 Temp. Control/Temp. Wet Ice 0.4 Direction / Handled By RECEIVED AMMERMAN, MARK Container# f C0018562 : C0018610 ' C0018615 C0018619 Gross Weight pH Container Type 652.7 g 500 ml Clear Plastic 618.6 g 500 ml Clear Plastic 614.7 g 500 ml Clear Plastic 598.8 g 500 ml Clear Plastic Preservative NONE NONE NONE NONE Mfg. Lot 3232010 3232010 3232010 3232010 Mfg. ID 471372 471599 471604 471608 Miscellaneous Item Key None Description ICOC 1: ' Sample ID L0001445-0001 jr^LOO01445-0002 ' L0001445-0003 ' L0001445-0004 n Matrix LIQUID SOLID LIQUID LIQUID Fraction Water Soil/Sludge Water Water Samples Sample DAI-121003-NW-01 DAI-121003-NW-02 DAI-121003-NW-03 DAI-121003-NW-FB Date Sampled Date Received 12/11/2003 12/12/2003 12/11/2003 12/12/2003 12/11/2003 12/12/2003 12/09/2003 12/12/2003 Date Due 12/26/2003 12/26/2003 12/26/2003 12/26/2003 i 2/12/2003 ' Login, rpt Report Version: Dec 12 2003 11:28AM Page 1 of 2 000332 Instance: R0076088 R0076088 ^0001445-0001 Container ^*1 C0018615 / 500 ml Clear Plastic / NONE if -- L0001445-0002 P < Container ' . CO018562 / 500 ml Clear Plastic / NONE ^0001445-0003 ` Container C0018610 / 500 ml Clear Plastic / NONE n 0001445-0004 f * . Container t 1 C 0018619/500 ml Clear Plastic/NONE Bottles Method Method Method Method r ^ l 2/12/2003 I Login.rpt Report Version: Dec 12 2003 11:28AM Page 2 of 2 000333 Instance: R0076088 R0076088 Composite Number of Containers 000334 RESEARCH PROJECT INFORMATION CHAIN O F CUSTODY/ANALYSIS REQUEST FORM 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 ii LPage _ _ L _ f - ANALYSES REQUESTED Client (name & address): _____ (ikid/. f & r 5 /4 4 dock? xAscsXJ Phone: Fax: Sampler: Project Manager (Name & E-mail Address): ____ ' - I _____ 1 ----------------------------------------------------------------------------- Ifa /S a/z& sz1 / I 3s-<k><( 1Project Name: / `----- / PFoA- s-hzL' RO. #: //> o 3 o z 3 3 D Quotation #: Please fill out this form completely to ensure correct analysis and proper handling of your samples. SAMPLE ANALYSIS ExyLIMS# Client Sample Identification S2Collection Collection oDate Time i Specify Matrix ' AI- /V 0 O 3 'AH>' <3/ /2-/>3 /Z Z S X JL {jJoJ-e-r b /ZJOO3 iZ -fo J /Z jTO AAb/ZitiS -/VU) - 0 3 OYO X T S/uZ, X _ L t.ltr Comments t/cJie U/asJem-br UA/skrs U. J J r tOOlJ _K_ 33 V Ai-Zloca -//U)- F A /Z- 7-o O30 2<L I T Ci/cjbr LAB USE ONLY X __ __ j ii 11 R E C IP IE N T : P E E L H ER E 000335 USA A irb ill Express AMDS 3 f l b l `b'MFedEx Tracking Number 1 From ThisportioncaneeremovedforRecipient'srecords. Date / f / i m i FedEx Tracking Number flH053flfc.ltib44 Sen,ddeerr'-ss' J V '*%/) j ; n (L Namn8e , , y v i l # I ' A. I i , Phone TO O Company k` i l K l i E R IC A I M ; h r.,- 1 ? iJ : ;s v . J E I S m xm m m ve 'SdSW mi1-. U kaqe Service Packages up to 150lbs. QeBvery cypmitmentmaybelater insomeareas. 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Ji-M., i\Z2 l : Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site: NA L1445 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 Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: 123003C Karen Risha LC/MS/MS Unit # 7 12/30/03 01/01/04 Exygen ID XC123003-0 XC123003-I X C 123003-2 XC123003-3 XC123003-4 XC123003-5 XC123003-6 Methanol Wash 0106020 Control L1445-4 0106020 Spk A 0106020 Spk B XC123003-1 XC123003-2 XC123003-3 L1445-1 Spk C L1445-1 . . L1445-1 Rep L1445-3 XC123003-4 XC123003-5 XC123003-6 ' Sponsor ID NA DAI-121003-NW-FB NA NA - DAI-121003-NW-01 DAI-121003-NW-01 DAI-121003-NW-01 DAI-121003-NW-03 - - Sample Code c CS CS CS CS CS CS c c c LCS LCS CS CS CS LF S S S CS CS CS Run No. 123003C-401 123003C-402 123003C-403 123003C-404 123003C-405 123003C-406 123003C-407 123003C-408 123003C-409 123003C-410 123003C-411 123003C-412 123003C-413 123003C-414 123003C-415 123003C-416 123003C-417 123003C-418 123003C-419 123003C-420 123003C-421 123003C-422 Std. Cone. (ng/L) 0 25 50 100 250 500 1000 25 50 100 250 500 1000 PFOA Found (ng/L) = (peak area - intercept) / slope x DF Recovery (%)= ______[PFOA found (ag/L)-PFQA found in control (ng/L)]_____ x 100 amount PFOA added (ng/L) Dilution Factor - - - - 1 1 1 1 1000 1000 1000 1000 - - Peak Area 0 7317 14700 28999 70098 142255 282552 232 0 79865 13478 134854 7172 14598 28567 171988 19324 18194 378663 70050 140888 281215 PFOA Found (ng/L) - - ND 282 46.7 478 609.000 67.400 63400 * - Amount PFOA Added (ng/L) - 50 500 500000 - Recovery (%) . . - - - 93 96 108 - --- Standard Curve : Linear (1/x weighted) Intercept = 337.718 Slope = 281.652 Coef. Of D et = 0.999969 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 LOD NQ = Not quantifiable = Response between LOD and LOQ *Sample requires further dilution. See data set 123003CR. Spreadsheet prepared by: 000 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 Internal Chain of Custody/Fortification Sheet Exygen Study Number: L1445 Matrix: Water Sponsor Study/Protocol No: NA The samples listed below were removed from refrigerator No. 3 k - Time 6 1 3 0 Date Jj 3 0 CLIENT SAMPLE ID EXYGEN ID NUMBER VOLUME (mL) FORTIFICATION (ng) na 0106020 Control 40.0 - r~< i na 0106020 Spk A 40.0 2.0 na 0106020 SpkB 40.0 20.0 DAI-121003-NW-01* L1445-1 SpkC 40.0 20000.0 DAI-121003-NW-01* L1445-1 40.0 _ DAI-121003-NW-01* L1445-1 Rep 40.0 - DAI- 121003-NW-03* L I 445-3 40.0 - DAI-121003-NW-FB L I445-4 40.0 - - - -- - - -- - - -- - - -- n- - - -- -- - - -- fl i' - - -- -- -- - - -- - - -- 0106020 Spk A 0106020 SpkB L1445-1 SpkC - Spiking Solution Used F120903-5 (10 ng/mL) F120903-4 (100 ag/mL) F120903-1 (100000 ng/mL) _ Volume Used for Spiking 200 (iL (200 pL micropipet) 200 pL (200 |jL micropipet) 200 pL (200 |iL micropipet) - Initial/Date b / !2 30|c>- w ! ' 'I2|30b- Hr - - -- H _ _ -- _ _ -- All samples were measured: n Time OQOO______ D ate_L2^3cJj}3___ Initials '2-' After measuring samples were returned to refrigerator No. Time lOOO Date /zj-injfiSi Initials Comments: 200 pL of 250 mg/mL sodium thiosulfate was added to all samples before spiking. Initials/Date: J /2 f .3 o /A 5 ^Sample was diluted lOOOx times before extraction. Spiking was done using a 40 mL sample before dilution. Analysis Summary: Data Set: I2SCDS>C Data Set: 1 Data Set: _____ 2 Initials/Date: Initials/Date: Initials/Date: / I2|2>l)p3> /Off* Set extraction/analysis data verified by: `- F Date: / July 26,2001/6 000336 0 000337 1 ::::3 td :TMi " '"J ... :i 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: L1445 MATRIX: Water METHOD: $$ ANALYTES: PFOA PROTOCOL NUMBER: NA Client ID na na na DAI-121003-NW-01* Exygen ID 0106020 Control 0106020 Spk A 0106020 Spk B L1445-1 Spk C STEP 1 STEP 2 DAI-121003-NW-01* L1445-1 DAI-121003-NW-01* L1445-1 Rep DAI-121003-NW-03* DAM21003-NW-FB - L1445-3 L I445-4 - \V \V -- - - -- - - -- - - -- _ - -- - - -- . - -- _ - -- . - -- _ - -- - - -- - - -- _ - -- _ - -- - - -- *lnitials/Date Z - /folA5 rzfsnbs. STEP 1: SPE column clean-up STEP 2: Final volume to 5 mL collected in 15 mL polypropolene tubes STEP 3: LC/MS/MS analysis STEP 4: LC/MS/MS reanalysis. Dilutions (mL/mL) -- ^ -- -- -- -- - - - STEP Dilutions (mL/mL) __ STEP 4 -- <*- XT - - - - - -- _ - ry _CL - - - - ' - A Reagents/ Materials Methanol C18SPE Type I Water . _ . - Initials/Date - Lot# a NA - cjx nisoo 1 - - - - HPLC - - Methanol Ammonium Acetate Type I water - 1 _____ NA j;- Initials/Date 1 & Initials and date under each step indicates the personnel that performed this step. $$ Method of Analysis for the Determination of Perfluorooctane sulfonate (PFOS), Perfluorooctane sulfonylamide (PFOSA), and Perfluorooctanoate (POAA) in Water COMMENTS: Final extracts stored in refrigerator Initials: C. Date: July 19,2001/4 n ... ! ; ' 1 ') ; :z 1 1 : ii i 3 ' n ': n 3 3 7 T l 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 PREPARATION OF EXTRACTED CALIBRATION STANDARDS Exygn study n o . JJL-- 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 Exygei) Sample .ID 0106020 Sample Description Type I WaterA Fort. Solution ID - Fort. Soin. Cone. (ng/mL) Fort Volume <UL) Micropipet used (uL) - -- Fort. Level fppt) - Final Solution ID #** XC123003-0 Reagents/ Materials Methanol Lot# HS30834S NA 0106020 Type I Water*' F120903-5 10 100 200 25 XC123003-1 C18 SPE NA 0106020 Type I Water* F120903-5 ` 10 200 200 50 XC123003-2 Type I Water NA NA 0106020 Type I Water* F120903-5 10 400 200 100 XC123003-3 - _ NA 0106020 Type I Water* F120903-4 100 100 200 250 XC123003-4 - - NA 0106020 Type I Water* F120903-4 100 200 200 500 XC123003-5 - - NA 0106020 Type I Water* F120903-4 100 400 200 1000 XC123003-6 - - NA 0106020 Type I Water* F102703-2 100 100 200 250 XC123003-7 ~ 3 r~ tzj3o]o3>- - - - - - - - Initials/Date: Vertical arrows in a column indicate identical values. **This must be a unique number. Use this system: Extracted Calibration Soln ID #: XCMMDDYY-0,1,2,3. etc. Samples removed from(fefrigeratQpy freezer # 32- Time: 40 mL of each sample measured using a *30 mL graduated cylinder. After measuring, samples returned to ^ rig e ra tp / freezer # 3 2 - Time: Samples fortified: SPE clean-up: Initials/Date: Initials/Date: !2M <3 Final volume adjusted to 5 mL: Initials/Date: Initials/Date:. Initials/Date: Initials/Date: / |30| ( f , |3 i|3 o | ( a T H IS IS AN EXACT COP Y OF THE ORIGINAL DOCUMENT.* DATE. ) 2 h i[ b 3 Extracts placed in refrigerator # 3 2 - Initials/Date: STANDARD EXPIRATION DATE: 1/13/04 Comments: AThis type I water has been filtered through a hypercarb filter * Method of Analysis for the Determination of Ammonium Perfluorooctanoate (APFO) in Water. July 10,2001/0 00 00033 n z " : z ..i i ::::i :i z i j :* n Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochem; iPRO\SampleDB\123003C Daikin Water.spl Printed: Wed Dec 31 10:41:50 2003 L jP I2I 3 I I & 3 _____________________ Vial File Name LIMS ID Client ID Sample Description 1 1 123003C-401 ___ XC123003-0, 0 ng/L standard 2 2 123003C-402 -- -- XC123003-1, 25 ng/L standard 3 3 123003C-403 -- -- XC123003-2, 50 ng/L standard 4 4 123003C-404 -- -- X C 123003-3, 100 ng/L standard 5 5 123003C-405 -- -- XC123003-4, 250 ng/L standard 6 6 123003C-406 -- -- XC123003-5,500 ng/L standard 7 7 123003C-407 -- -- XC123003-6,1000 ng/L standard 8 92 123003C-408 -- -- Methanol Wash 9 51 123003C-409 -- -- 0106020 Control 10 52 123003C-410 -- -- L1445-4 11 53 123003C-411 -- -- 0106020Spk A, 50 ng/L 12 54 123003C-412 -- -- 0106020 Spk B, 500 ng/L 13 2 123003C-413 -- -- XC123003-1, 25 ng/L standard 14 3 123003C-414 -- -- XC123003-2, 50 ng/L standard 15 4 123003C-415 -- -- XC123003-3,100 ng/L standard 16 55 123003C-416 -- -- L1445-1 Spk C, 500000 ng/L, DF=1000 17 56 123003C-417 -- -- L1445-1, DF=1000 18 57 123003C-418 -- -- L1445-1 Rep, DF=1000 19 58 123003C-419 -- -- L1445-3, DF=1000 20 5 123003C-420 -- -- X C 123003-4,250 ng/L standard 21 6 123003C-421 -- -- XC123003-5, 500 ng/L standard 22 7 123003C-422 -- -- XC123003-6,1000 ng/L standard 000339 "1 : 1 rra ' ri r r z:i .:i Exygen study NO. Page 1 Page Position: (1 ,1 ) Matrix Sample Type Cone (ng/L) C one(B) C on cC Test ID DF MS Method ___ Blank -- Standard -- Standard . . . Standard -- Standard -- Standard -- Standard -- - Blank -- Blank -- Analyte -- QC -- QC -- Standard -- Standard -- Standard -- QC -- Analyte -- Analyte -- Analyte -- Standard - - - Standard -- Standard 0 25 50 100 250 500 1000 -- -- -- 50 500 25 50 100 500000 -- -- -- 250 500 1000 ___ -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- --0 --0 --0 --0 --0 --0 --0 --0 --0 --0 --0 --0 --0 --0 --0 --0 --0 --0 --0 --0 --0 0------ 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA 1 008 PFOA } : ..; 1 i . - , :1 --j ::1 -} : : r i : - -j Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochems.PI SO\SampleDB\123003C Daikin Water.spl Printed: Wed Dec 31 10:41:50 2003 l HPLC Method MS Tune File Inj Volume (pL) 1 water PFOATune 15 2 water PFOATune 15 3 water PFOATune 15 4 water PFOATune 15 5 water PFOATune 15 6 water PFOATune 15 7 water PFOA Tune 15 8 water PFOATune 15 9 water PFOATune 15 10 water PFOATune 15 11 water PFOA Tune 15 12 water PFOATune 15 13 water PFOATune 15 14 water PFOATune 15 15 water PFOATune 15 16 water PFOATune 15 17 water PFOATune 15 18 water PFOATune 15 19 water PFOATune 15 20 water PFOATune 15 21 water PFOATune 15 22 water PFOA Tune 15 000340 ' } ; .... i ; : n : "i "* r ] "T l ........1 " Exygen STUDY NO. Page 2 Page Position: (2,1 ) m LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA [ Exvgen Study No: L1445 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #7) i Computer: COMPAQ Professional Workstation AP200 Software: Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 1 , Micromass Limited: MassLynx 3.4 Build 004 HPLC Equipment: Hewlett Packard (HP) Series 1100 HP Quat Pump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column: Genesis C-8, 5 cm x 2.1 m m i.d. x 4 jr (Exygen ID:MA10464) (JONESCHROMATOGRAPHY: Part No. FK5962EJ) Mobile Phase (A) : M obile Phase (B) : 2 mM Ammonium Acetate in Type I W ater M ethanol Analyst: Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 t NOTE: The next 3 pages are computer generated printouts from n the masslynx software program. The pages contain the instrument settings used for the analysis of this data set. n All H andw ritten P eak ID 's by: fc r~i ri k! \ n 000341 n n r< Scanning Method Report Method: C:\MASSLYNX\008 APPO. PRO\ACQUDB\008 PFOA k' f' Last Modified: Wed Mar 20 15:07:50 2002 r Printed: Wed Dec 31 11:09:49 2003 Solvent Delay ( mins ) : 0.00 p a llia Function : 1 MRM of 1 Mass Pair ( ESP- ) Inter Channel Delay ( Secs ) : Span ( Daltons ) : Start Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 8.00 1 Dwell (Secs) Coll Energy (eV) Cone ( V ) 1 413.00 369.00 0.20 10 10 Page 1 I if ! k. rt ii t, 000342 Method Report Method File: Last Modified: Printed: c :\masslynx\008 apfo.pro\acqudb\water Wednesday, December 31, 2003 11:02:02 Wednesday, December 31, 2003 11:10:02 HP1100 LC Pump Initial Conditions Solvents A% B% C% D% 60.0 40.0 0.0 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 0.300 15.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 10 entries which are : Time 0.00 0.40 1.00 7.00 7.50 9.00 9.50 13.50 14.00 15.00 A% 60.0 60.0 10.0 10.0 0.0 0.0 60.0 60.0 60.0 60.0 B% 40.0 40.0 90.0 90.0 100.0 100.0 40.0 40.0 40.0 40.0 C% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 D% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 0.400 0.400 0.400 0.300 0.300 Page 1 \2 |3 l|b ^ Pressure 400 400 400 400 400 400 400 400 400 400 HP1100 LC Pump External Event Timetable The Timetable contains 4 entries which are : Time Initial 0.00 0.10 8.00 Column Switch Off Off Off Off Contact1 Off On Off Off Contact2 Off Off On Off Contact3 Off Off Off Off Contact4 Off Off Off Off HP1100 Autosampler Initial Conditions Draw Speed Eject Speed ( f j . 1/min) Draw Position (mm) Stop Time (mins) Injection Volume ( x l ) Vial Number . 200.0 200 0.10 15.00 15.0 92 000343 Tuning Method Report Method: C:\MASSLYNX\008 A PFO.PRO\ACQUDB\PFOA TUNE Printed: fn Wed Dec 31 11:10:20 2003 *n t r$* , Page 1 ! n SOURCE ( ESP- ) 1: Capillary Cone r". Hexapole 1 1 ! Aperture 1 Hexapole 2 Source Block Temp. i i Desolvation Temp. bi ti1e ~:.- Pressures rn Analyser Vacuum k - Gas Cell Set Rdbk 3.00 10 0.0 0.0 0.0 100 300 -2.93 -10 101 300 Rdbk OFF 3. Oe- 3 Analyser LM Res 1 ' HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas Flows Cone Gas Desolvation Set Rdbk 14.0 14.0 1.0 -2 10 2 14.0 14.0 2.0 700 8 9 11 -695 Rdbk 87.8 708.8 n pi 000344 c? I ! Quantify Calibration Report Study No.:L1445, Set No.:123003C, Ext .Date:12/30/03, Analyst :K.Ri sha Page 1 O Exygen Research, 3058 Research Drive, State College, PA 16801 000345 n I 1 Quantify Sample Report Study No.:Ll445, Set No.:123003C, Ext.Date:12/30/03, AnalystsK.Risha Page 1 lr .1 Sample List: p:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\123003C Daikin Water Last modified: Wed Jan 07 07:42:48 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Mon Dec 22 10:23:22 2003 n Job Code: Initials I1 Printed: Wed Jan 07 07:46:00 2004 D a te ...Q l\L n ,,l,-,, ,,,----------- -------------- R u n # \ i ^ D ^ f e \ To I Name: 123003C-401 Text : 'ft ! l' ft I ( f' 1 Exygen Research, 3058 Research Drive, State College, PA 16801 {H 000346 n ! Quantify San>le Report Study No.:L1445, Set N o . :123003C, Ext.Date:12/30/03, AnalystsK.Risha Page 2 fl Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\123003C Daikin Water pi Last modified: Wed Jan 07 07:42:48 2004 ` Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Mon Dec 22 10:23:22 2003 jH Job Code: Ij Printed: . Wed Jan 07 07:46:00 2004 n Name: 123003C-402 Text: b- J> JP-"! M' ri - \ m ' .. ... ,, ,w. ,,, ,- ^ Exygen Research, 3058 Research Drive, State College, PA 16801 000347 Quantify Sample Report Study No.:L1445, Set No.:123003C, Ext.Date:12/30/03, AnalystiK.Risha Page 3 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\123003C Daikin Water Last modified: Wed Jan 07 07:42:48 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Mon Dec 22 10:23:22 2003 Job Code: Printed: Wed Jan 07 07:46:00 2004 Name: 123003C-403 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000348 Quantify Sample Report Study No.:L1445, Set No.:123003C, Ext.Date:12/30/03, Analyst sK.Risha Page 4 jH Sample List: P;\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\123003C Daikin Water I ' Last modified: Wed Jan 07 07:42:48 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Mon Dec 22 10:23:22 2003 fTM Job Code: M Printed: Wed Jan 07 07:46:00 2004 Name: 123003C-404 Text: 1 : PFOA t! t: fi . !,! n ! "i tJ H ii Exygen Research, 3058 Research Drive, State College, PA 16801 000349 Quantify Sample Report Study No.:L1445, Set No.:123003C, Ext.Date:12/30/03, Analyst:K.Risha Page 5 p*j Sample List: P: \Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\123003C Daikin Water I Last modified: Wed Jan 07 07:42:48 2004 ** Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PF0Al00203 Last modified: Mon Dec 22 10:23:22 2003 Job Code: eu .. . . , ... ... ,, 1 J Printed: Wed Jan 07 07:46:00 2004............ n Name: 123003C-405 Text: 1 : PFOA XC123003-4, 250 ng/L standard 123003C -405 Sm (Mn, 2x2) I1 100i I*"! ii %: 01-Jan-2004 01:40:07 LC/MS/MS #7 M RM of 1 Channel ES413 >369 7.41e5 Area 0 'r ~ I t I l I 1 I [1-- r I T - |- T - | I I l' - l - ' l I T - J - I I I "" T I I " I1"I-- I I T T |-H 1.00 2.00 3 .0 0 4.00 M ' ' " 1 1 1 1 ....................... T im e 6 .0 0 7.00 8.00 L i ,i jpw ti n Exygen Research, 3058 Research Drive, State College, PA 16801 000350 Quantify Sample Report Study No.:L1445, Set No.:123003C, Ext .Date:12/30/03, Analyst:K.Risha Page 6 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\123003C Daikin Water Last modified: Wed Jan 07 07:42:48 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Mon Dec 22 10:23:22 2003 Job Code: Printed: Wed Jan 07 07:46:00 2004 Name: 123003C-406 Text: 1: PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000351 Quantify Sample Report Study No.:L1445, Set No.:123003C, Ext.Date:12/30/03, Analyst:K.Risha Page 7 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\123003C Daikin Water Last modified: Wed Jan 07 07:42:48 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Mon Dec 22 10:23:22 2003 Job Code: Printed: Wed Jan 07 07:46:00 2004 Name: 123003C-407 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000352 Quantify Sample Report Study No.:L1445, Set No.:123003C, Ext.Date:12/30/03, Analyst:K.Risha Rage 8 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\123003C Daikin Water Last modified: Wed Jan 07 07:42:48 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Mon Dec 22 10:23:22 2003 Job Code: Printed: Wed Jan 07 07:46:00 2004 Name: 123003C-408 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000353 Quantify Sample Report Study No.:L1445, Set No.:123003C, Ext.Date:12/30/03, Analyst:K.Risha Page 9 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\123003C Daikin Water Last modified: Wed Jan 07 07:42:48 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochezns.PRO\MethDB\PFOA 100203 Last modified: Mon Dec 22 10:23:22 2003 Job Code: Printed: Wed Jan 07 07:46:00 2004 Name: 123003C-409 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000354 n ; Quantify Sanale Report Study No.:L1445, Set No.:123003C, Ext.Date:12/30/03, Analyst:K.Risha Rage 10 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\123003C Daikin Water H Last modified: Wed Jan 07 07:42:48 2004 f Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Mon Dec 22 10:23:22 2003 Tl Job Code : Printed: Wed Jan 07 07:46:00 2004 I I Name: 123003C-410 Text : 1 : PFOA 0*^ ;? i- n * * Exygen Research, 3058 Research Drive, State College, PA 16801 i 000355 Quantify Sample Report Study No.:L1445, Set No.:123003C, Ext.Date:12/30/03, Analyst:K.Risha Rage 11 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\123003C Daikin Water Last modified: Wed Jan 07 07:42:48 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Mon Dec 22 10:23:22 2003 Job Code: Printed: Wed Jan 07 07:46:00 2004 Name: 123003C-411 Text : 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000356 n I Quantify Sample Report r Study No-:L1445, Set No.:123003C, Ext.Date:12/30/03, Analyst:K.Risha Page 12 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\123003C Daikin Water || Last modified: Wed Jan 07 07:42:48 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Mon Dec 22 10:23:22 2003 f"; Job Code: Printed: Wed Jan 07 07:46:00 2004 Name: 123003C-412 ' Text : 1 : PFOA 0106020 Spk B, 500 ng/L 123003C -412 Sm (Mn, 2x2) 10Ch %- r* V ., 1.00 2.00 5.25 134854 3.00 )""l |" l l - l l - [ l i f t 4.00 5.00 01-Jan>2004 03:37:12 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1 .40e6 Area 6.00 7.00 T im e 8.00 \ tt j t* i fl ki Exygen Research, 3058 Research Drive, State College, PA 16801 000357 Quantify Sample Report Study No.:L1445, Set No.:123003C, Ext.Date:12/30/03, Analyst:K.Risha Page 13 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\123003C Daikin Water Last modified: Wed Jan 07 07:42:48 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Mon Dec 22 10:23:22 2003 Job Code: Printed: Wed Jan 07 07:46:00 2004 Name: 123003C-413 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000358 f ; Quantify Sanale Report Study No.:L1445, Set No.:123003C, Ext.Date:12/30/03, AnalystsK.Risha Page 14 #"> Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\123003C Daikin Water | , Last modified: Wed Jan 07 07:42:48 2004 1 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Mon Dec 22 10:23:22 2003 n Job Code: f- ' i Printed: Wed Jan 07 07:46:00 2004 ............. 1 " 1 1 --'-- ---- ----- --- r ---- -- -- ---- - - " ., .... - " I i Name: 123003C-414 Text: f. ! ; fT k4 n Exygen Research, 3058 Research Drive, State College, PA 16801 000359 i , Quantify Sandle Report r Study No.:L1445, Set No.:123003C, Ext.Date:12/30/03, AnalystsK.Risha Page 15 r* Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\123003C Daikin Water Last modified: Wed Jan 07 07:42:48 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Mon Dec 22 10:23:22 2003 pi Job Code: I. ' . . . .' Printed: Wed Jan 07 07:46:00 2004 ' " - f* I Name: 123003C-415 Text: ' ft f' l, i) Exygen Research, 3058 Research Drive, State College, PA 16801 000360 Quantify Sample Report Study No.:L1445, Set No.:123003C, Ext.Pate:12/30/03, AnalystrK.Risha Page 16 f~r Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\123003C Daikin Water I ! Last modified: Wed Jan 07 07:42:48 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Mon Dec 22 10:23:22 2003 n Job Code : &.4 Printed: Wed Jan 07 07:46:00 2004 Name: 123003C-416 Text : 1 : PFOA L1445-1 Spk C, 500000 ng/L, DF=1000 12 3 0 0 3 C -4 1 6 Sm (Mn, 2x2) 1 0Ch %: 01-Jan-2004 04:43:59 LC/MS/MS #7 MRM of 1 Channel ES413 > 369 1.84e6 Area CF-f'i'-i r ir - j T - t ' I T ~ ] T T T T-- I 1r - ! 1 | -i . T r p r n - f r r 1.00 2.00 3.00 bi I' r 4.00 T im e- i - f - T - r - 1 - 1 - [- I n I ! n T I" f I I I I I 6 .0 0 7.00 8.00 Ii *t i \ *i Exygen Research, 3058 Research Drive, State College, PA 16801 000361 Quantify Sample Report Study No.:L1445, Set No.:123003C, Ext.Date:12/30/03, Analyst:K.Risha Page 17 r*- Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\123003C Daikin Water i Last modified: Wed Jan 07 07:42:48 2004 1 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Mon Pec 22 10:23:22 2003 Job Code: Printed: Wed Jan 07 07:46:00 2004 m f Name: 123003C-417 Text : 1 tS t , I: f""* 1* f5 fs I; Exygen Research, 3058 Research Drive, State College, PA 16801 f*"; 000362 i* ; Quantify Sample Report r Study No.:L1445, Set No.:123003C, EKt.Date:12/30/03, AnalystrK.Risha Page 18 f"' Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\123003C Daikin Water Last modified: Wed Jan 07 07:42:48 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Mon Dec 22 10:23:22 2003 75 Job Code: f '( i Printed: Wed Jan 07 07:46:00 2004 Name: 123003C-418 Text: I' !'j r-i f: ; I M ii Li,, J-i Exygen Research, 3058 Research Drive, State College, PA 16801 n 000363 * i Quantify Sample Report Study No.:L1445, Set No.:123003C, Ext.Date:12/30/03, Analyst:K.Risha Page 19 f*i Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SanipleDB\123003C Daikin Water I* Last modified: Wed Jan 07 07:42:48 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Mon Dec 22 10:23:22 2003 F""S Job Code: Printed: Wed Jan 07 07:46:00 2004 rj Name: 123003C-419 Text: 1 : PFOA L1445-3, DF=1000 t, i 12 3 0 0 3 C -4 1 9 S m (Mn, 2 x 2 ) 1 0 0 -i J*--1 %: 5 .2 3 3786631 1 1 01-Jan-2004 05:34:04 LC/MS/MS #7 MRM of 1 Channel ES413 >369 3.98e6 Area n 0 : LT " i t" t [ "1 --j "1 - 1 j - 1 - n T" j i --i " r r T ' i --r i t i f i t i - t t - i l i f f i r i j i r r " f T""7--! ..t--i i i i l i- i T - i i - i 11 i n r i --r i n T " i --r 1i r 1 T i m e 1.00 2.00 3 .0 0 4.00 5.00 6.00 7.00 8.00 n ti f*5 fl yi Exygen Research, 3058 Research Drive, State College, PA 16801 i 000364 n f Quantify Sample Report Study No.:L1445, Set No.:123003C, Ext.Date:12/30/03, Analyst:K.Risha Page 20 p' Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\123003CDaikin Water I Last modified: Wed Jan 07 07:42:48 2004 : Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Mon Dec 22 10:23:22 2003 n Job Code: Printed: Wed Jan 07 07:46:00 2004 Name: 123003C-420 Text: 1 : PFOA ti XC123003-4, 250 ng/L standard 12 3003C -420 Sm (Mn, 2x2) 100] fc' ' % - H i~ i t-: ' 1.00 2.00 3 .0 0 ir \ I -! * T I T " I I- 1 4.00 5.24 5 .0 0 01-Jan-2004 05:50:49 LC/MS/MS #7 MRM of 1 Channel ES413 >369 7.55e5 Area | T im eT - T - p i - 1 - r- T ! I "I I r - | I I I I II m I 6.00 7.00 8.00 I" l; Exygen Research, 3058 Research Drive, State College, PA 16801 000365 pm I :i |4 Quantify Sample Report : Study No.:L1445, Set No.:123003C, Ext.Date:12/30/03, Analyst:K.Risha Page 21 Saatple List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\123003C Daikin Water _ Last modified: Wed Jan 07 07:42:48 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Mon Dec 22 10:23:22 2003 Job Code: ' Printed: Wed Jan 07 07:46:00 2004 ; ; Name: 123003C-421 Text : n 1: PFOA____________ _____________________________________________________________________________ , XC123003-5, 500 ng/L standard 01-Jan-2004 06:07:34 LC/MS/MS #7 123003C-421 Sm (Mn, 2x2) 100-1 5.24 140888 MRM of 1 Channel ES413 >369 1,49e6 n Area %- 0^ f "*, s! 1.00 'I I *T '''I 1 1 1 `"1 2.00 3 .0 0 4.00 5.00 t i " I I ' 1 I I I " 1m " 1 I I Tim e 6.00 7 .0 0 8.00 w. k1 f: 1 ! I(-, . I' r; Exygen Research, 3058 Research Drive, State College, PA 16801 000366 Quantify Sample Report Study No.:L1445, Set No.:123003c. Ext.Date:12/30/03, Analyst:K.Risha Page 22 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.FR0\SampleDB\123003C Daikin Water Last modified: Wed Jan 07 07:42:48 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Mon Dec 22 10:23:22 2003 Job Code: Printed: Wed Jan 07 07:46:00 2004 Name: 123003C-422 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000367 I RAW DATA REPORT H Sponsor Study No: NA Exygen Study No: L1445 Analyte: PFOA Ions Monitored: 413->369 r~i Site: HA Limit of Quantitation: Injection Volume: Matrix: Sample Volume: Final Volume: 50 ng/L 15 pL Water 40.0 mL 5.0 mL Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: 123003CR Karen Risha LC/MS/MS Unit # 7 12/30/03 01/07-08/04 t' Amount Std. PFOA PFOA n Exygen ID Sponsor ID Sample Code Run No. Cone. Dilution <np/L) Factor Peak Area Found (ng/L) Added (ng/L) Recovery m in XC123003-0 - C 123003CR-501 0 - 0 - - - X C 123003-1 - CS 123003CR-502 25 - 6837 - - - gmm, XC123003-2 XC 123003-3 - CS 123003CR-503 50 - 14068 - - - - CS 123003CR-504 100 - 28579 - - - XC123003-4 - CS 123003CR-505 250 - 68648 - - - XC123003-5 - CS 123003CR-506 500 - 139034 - - - XCI23003-6 - CS 123003CR-507 1000 - 286990 - - - Methanol Wash - C 123003CR-508 - - 282 - - - L1445-3 DAI-121003-NW-03 S 123003CR-509 - 10000 16812 599000 - - XC 123003-3 - CS 123003CR-510 100 - 29626 - - - XC123003-4 - CS 123003CR-511 250 - 68631 - - - f- PFOA Found (ng/L) = (peak area - intercept) / slope x DF Recovery (%) ~ IPFOA found (ng/L)-PFOA found in control (ng/L)] x 100 amount PFOA added (ng/L) n Standard Curve : Linear (1/x weighted) Intercept = -127.069 Slope = 282.826 Coef. Of Det. = 0.999457 CS = Calibration standard C = Control sample S = Sample h. LF = Lab fortified sample FF = Field fortified sample LCS s=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: ^ _ / _ a i _ N p q te 1 I5 H f. ; nsi j ki % tj r-i 1s 1 p ! i i 1 D1 Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochems 3RO\SampleDB\123003CR Daikin Water.spl Printed: Wed Jan 07 10:17:09 2004 |bl|oL|______________________ Exygen STUDYNO* -- nd ID Page 1 Page Position: (1 ,1 ) Vial File Name LIMS ID Client ID Sample Description Matrix Sample Type Cone (ng/L) Cone (B) Cone C Test ID DF MS Method 1 1 123003CR-501 2 2 123003CR-502 -- 3 3 123003CR-503 -- 4 4 123003CR-504 -- 5 5 123003CR-505 -- 6 6 123003CR-506 -- 7 7 123003CR-507 -- 8 92 123003CR-508 -- 9 87 123003CR-509 -- 10 4 123003CR-510 -- 11 5 123003CR-511 -- -- -- -- -- -- -- -- -- -- -- XC123003-0, 0 ng/L standard XC123003-1,25 ng/L standard XC123003-2, 50 ng/L standard X C 123003-3,100 ng/L standard -- XC123003-4, 250 ng/L standard -- XC123003-5, 500 ng/L standard - XC123003-6,1000 ng/L standard -- Methanol Wash L1445-3, DF=10000 XC123003-3,100 ng/L standard -- X C 123003-4, 250 ng/L standard -- Blank Standard Standard Standard Standard Standard Standard Blank Analyte Standard Standard 0 25 50 100 250 500 1000 -- ... 100 250 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 10 008 PFOA 0 1 008 PFOA 0 1 008 PFOA 000369 ] ' : n ' m :r::i T1 j Masslynx - Sample List Sample List: C:\MASSLYNX\Flaoroche :s.PRO\SampleDB\123003CR Daikin Water.spl Printed: Wed Jan 07 10:17:09 2004 HPLC Method MS Tune File Inj Volume (pL) 1 water PFOATune 15 2 water PFOATune 15 3 water PFOATune 15 4 water PFOATune 15 5 water PFOATune 15 6 water PFOATune 15 7 water PFOATune 15 8 water PFOATune 15 9 water PFOATune 15 10 water PFOATune 15 11 water PFOATune 15 000370 Exygen STUDYHO* Page 2 Page Position: (2 ,1 ) i l3 Scanning Method Report r? Method: C :\MASSLYNX\FLUOROCHEMS .PRO\ACQUDB\008 PFOA Last Modified: Thu Oct 02 13:56:38 2003 - Li Printed: Wed Jan 07 10:17:14 2004 H Solvent Delay ( mins ) : 0.00 Function : 1 MRM of 1 Mass Pair ( ESP- } Inter Channel Delay Span ( Daltons ) : Start Time ( Mins ) End Time ( Mins ) : Repeats : Channel Parent Secs ) : Daughter 0.03 0.00 0.00 8.00 1 Dwell (Secs) Coll Energy (eV) Cone ( V ) 1 413.00 369.00 0.20 10 10 Page 1 n jtfr"?` n R! : \ n 000371 ) n ----------- 11 Method Report Method File: f| Last Modified: f1 ' " Printed: c :\masslynx\fluorochems .pro\acqudb\water Wednesday, January 07, 2004 10:02:38 Wednesday, January 07, 2004 10:17:19 t , % i( HP1100 LC Pump Initial Conditions Solvents A% f-4 B% C% D% 60.0 40.0 0.0 0.0 I** Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) t, Oven Temperature Right(C) 0.300 15.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable {1 The gradient Timetable contains 10 entries which are : Time H 0..00 t 0 .40 1..00 7 .00 ?-- ) 7 .50 9 .00 l'j 9 .50 13 .50 n 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 : D% 0. 0 0. 0 0. 0 0. 0 0 .0 0. 0 0. 0 0. 0 0. 0 0 .0 Time FT* Initial t 0.00 0.10 8.00 Column Switch Contactl Off Off Off On Off Off Off Off f* <: ! j HP1100 Autosampler Initial Conditions Contact2 Off Off On Off Contact3 Off Off Off Off Draw Speed jbJ Eject Speed (il/min) * Draw Position (mm) ` Stop Time (mins) Injection Volume (jul) Vial Number i- : 200.0 200 0.10 15.00 15.0 7 Flow 0 .300 0..300 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 r r n 000372 Tuning Method Report Method: C :\MASSLYNX\FLUOROCHEMS .PRO\ACQUDB\PFOA TUNE Ijj Printed: Wed Jan 07 10:17:29 2004 *!' Page 1 tn < 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 -10 100 300 Pressures Analyser Vacuum Gas Cell ""5 i`i .-i Rdbk OFF 3.2e-3 Analyser LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas Flows Cone Gas Desolvation Set Rdbk 14.0 14.0 1.0 -2 10 2 14.0 14.0 2.0 700 8 9 12 -695 Rdbk 87.8 707.3 000373 fl li Quantify Calibration Report Study No.:L1445, Set N o . :123003CR, Ext.Date:12/30/03, Analyst:K.Risha Page 1 Exygen Research, 3058 Research Drive, State College, PA 16801 000374 Quantify Sample Report Study No.:L1445, Set No.:123003CR, Ext.Date:12/30/03, Analyst:K.Risha Page 1 Sample List: Last modified: Method: Last modified: Job Code: Printed: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\123003CR Daikin Water Thu Jan 08 07:47:41 2004 P :\Data\LCMSMS7\Mas slynx\Fluorochems.PRO\MethDB\PFOA 100203 Mon Dec 22 10:23:22 2003 Au) Thu Jan 08 07:49:05 2004 Initials. D ate. Ann* t23&3&-501 To 03C65CR~5lL Name: 123003CR-501 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000375 Quantify Sample Report Study No.:L1445, Set No.:123003CR, Ext.Date:12/30/03, Analyst:K.Risha Rage 2 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\123003CR Daikin Water Last modified: Thu Jan 08 07:47:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Mon Dec 22 10:23:22 2003 Job Code: Printed: Thu Jan 08 07:49:05 2004 Name: 123003CR-502 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 000376 Quantify Sample Report ' Study No.:L1445, Set No.:123003CR, Ext.Date:12/30/03, Analyst:K.Risha Page 3 *n Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\123003CR Daikin Water |I Last modified: Thu Jan 08 07:47:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Mon Dec 22 10:23:22 2003 f*''- Job Code: Printed: Thu Jan 08 07:49:05 2004 Name: 123003CR-503 Text: 1 : PFOA XC123003-2, 50 ng/L standard 123003CR-503 Sm (Mn, 2x2) * -VH 100i %- 07-Jan-2004 23:08:43 LC/MS/MS #7 MRM of 1 Channel ES413 >369 9.31 e4 Area 0 0-1 1.00 I T -rrrj-r , ,v , 2.00 3.00 ' TT r m T r r ` I r ~ r ~r 4 .0 0 5 .0 0 6.00 7.00 Tim e 8.00 $ % \ fS 0*^ ll n Exygen Research, 3058 Research Drive, State College, PA 16801 i ! 000377 J Quantify Sample Report Study No.:L1445, Set No.:123003CR, Ext.Date:12/30/03, Analyst:K.Risha Page 4 r- Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\123003CR Daikin Water | | Last modified: Thu Jan 08 07:47:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A100203 Last modified: Mon Dec 22 10:23:22 2003 job Code: Printed: Thu Jan 08 07:49:05 2004 !? Name: 123003CR-504 ~ Text: v va '< tt. n ^* Exygen Research, 3058 Research Drive, State College, PA 16801 000378 Quantify Sample Report Study No.:1.1445, Set No.:123003CR, Ext.Date:12/30/03, Analyst:K.Risha Page 5 f** Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\123003CR Daikin Water f ! Last modified: Thu Jan 08 07:47:41 2004 V Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Mon Dec 22 10:23:22 2003 f2* Job Code: Printed: Thu Jan 08 07:49:05 2004 Name: 123003CR-505 Text: & 1 : PFOA \ J` XC123003-4, 250 ng/L standard 123003C R -505 Sm (Mn, 2x2) 100n 9 0/o: 0 rI' II I I' I ' i- p - i - n r I ! ' I I I I ' I.......'" i " i V, 't 1.00 2.00 3 .0 0 07-Jan-2004 23:42:05 LC/MS/MS #7 M RM of 1 Channel ES413 >369 4.80e5 Area 1 I ' I--' T-1 I I I I I I i h j i It t -| T im e 6.00 7.00 8.00 I! \ ii t1 if*" '<J Exygen Research, 3058 Research Drive, State College, PA 16801 000379 V Quantify Sample Report Study No.:L1445, Set No.:123003CR, Ext.Date:12/30/03, Analyst:K.Risha Page 6 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\123003CR Daikin Water ; ' Last modified: Thu Jan 08 07:47:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Mon Dec 22 10:23:22 2003 Job Code: Printed: Thu Jan 08 07:49:05 2004 Name: 123003CR-506 Text: n 1 : PFOA XC123003-5, 500 ng/L standard 123003CR-506 Sm (Mn, 2x2) 10Ch fs 5.15 139034 07-Jan-2004 23:58:52 LC/MS/MS #7 MRM of 1 Channel ES413 >369 9.26e5 Area s 0- 1.00 2.00 -r -r -p r -r -r - 3.00 "1--I----I--I--!--r 4.00 5.00 6.00 7.00 T -] Tim e 8.00 \/ n / Exygen Research, 3058 Research Drive, State College, PA 16801 000380 } a * Quantify Sample Report Study No.:Iil445, Set No.:123003CR, Ext.Date:12/30/03, Analyst:K.Risha Page 7 f * Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\123003CR Daikin Water ^1; Last modified: Thu <Jan 08 07:47:41 2004 - Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 ^ Last modified: Mon Dec 22 10:23:22 2003 f*. Job Code: v> Printed: Thu Jan 08 07:49:05 2004 ` Name: 123003CR-507 Text: 7 I 1: PFOA /**; tt i! I *\ 4f S r-3 Exygen Research, 3058 Research Drive, State College, PA 16801 000381 Quantify Sample Report Study No.:1.1445, Set No.:123003CR, Ext.Date:12/30/03, Analyst:K.Risha Page 8 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\123003CR Daikin Water '! ' Last modified: Thu Jan 08 07:47:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\MethDB\PF0A 100203 Last modified: Mon Dec 22 10:23:22 2003 Job Code: * Printed: Thu Jan 08 07:49:05 2004 Name: 123003CR-508 Text: M 1 : PFOA li i1 .f*i/ \ A Exygen Research, 3058 Research Drive, State College, PA 16801 000382 f * Quantify Sample Report ' Study No.:L1445, Set No.:123003CR, Ext.Date:12/30/03, Analyst:K.Risha Page 9 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\123003CR Daikin Water I Last modified: Thu Jan 08 07:47:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Mon Dec 22 10:23:22 2003 ^ Job Code: Printed: Thu Jan 08 07:49:05 2004 n' \ Name: 123003CR-509 " Text s 1 : PFOA ! i k1 lJ $ 'i . Exygen Research, 3058 Research Drive, State College, PA 16801 i; i- ', 000383 J Quantify Sample Report Study Ho.:1.1445, Set No.:123003CR, Ext.Date:12/30/03, Analyst:K.Risha Rage 10 f*. Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\SampleDB\123003CR Daikin Water . - Last modified: Thu Jan 08 07:47:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 ^ Last modified: Mon Dec 22 10:23:22 2003 f*- Job Code: Printed: Thu Jan 08 07:49:05 2004 Name: 123003CR-510 Text: r, i* i; f0? i4 0k- Exygen Research, 3058 Research Drive, State College, PA 16801 000384 f ~5 ; ; Quantify Sandle Report Study No.:L1445, Set No.:123003CR, Ext.Date:12/30/03, Analyst:K.Risha Page 11 Sample List: P:\Data\LCMSMS7\Masslynx\Fluorochems.PR0\SampleDB\123003CR Daikin Water : Last modified: Thu Jan 08 07:47:41 2004 Method: P:\Data\LCMSMS7\Masslynx\Fluorochems.PRO\MethDB\PFOA 100203 Last modified: Mon Dec 22 10:23:22 2003 P*1 Job Code: i ' ' Printed: Thu Jan 08 07:49:05 2004 Name: 123003CR-511 Text: 1 : PFOA XC123003-4, 250 ng/L standard p 123003C R -511 Sm (Mn, 2x2) >' i 100t ft %: 08-Jan-2004 01:22:06 LC/MS/MS #7 5.14 M RM of 1 Channel ES413 >369 4.79e5 Area 0 n I ! |-I" 1-1 T I I I i -T -p I I I I I I I I I I I I -I I I I I . 1.00 2.00 3.00 4.00 5 .0 0 i i ' ' t i ' i i ' "p'-iTi t rn i i Time 6.00 7 .0 0 8.00 t: \ : f"S jgrjkS i- !^ ! te ft Exygen Research, 3058 Research Drive, State College, PA 16801 000385 Sponsor Study No: Exygen Study No: Analyte: 1 ? Ions Monitored: Site: NA L1445 PFOA 413-> 369 NA R A W DATA REPORT Limit of Quantitation: Injection Volume: Matrix: Sample Weight: Final Volume: 50 ppt 15 pL Soil 5.0 g 5.0 mL Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: 011404A Karen Risha LC/MS/MS Unit #6 01/14/04 01/15-16/04 l- i Exygen ID r v XC011404-0 r XC011404-1 XC011404-2 XC011404-3 XC011404-4 f 8* XC011404-5 XC011404-6 Methanol Wash Reagent Blank Reagent Spk A f i Reagent Spk B XC011404-1 XC011404-2 XC011404-3 t L1445-2 Spk C L1445-2 L1445-2 Rep XC011404-4 ! XC011404-5 XC011404-6 Sponsor ID - - - - - - NA NA NA DAM21003-NW-02 DAH21003-NW-02 DAI-12I003-NW-02 - -' - Sample Code c CS CS CS CS CS CS c c ' LCS LCS CS CS CS LF s s CS CS CS Run No. 011404A-601 011404A-602 011404A-603 011404A-604 011404A-605 011404A-606 011404A-607 011404A-608 011404A-609 011404A-610 011404A-611 011404A-612 011404A-613 011404A-614 011404A-615 011404A-616 011404A-617 011404A-618 011404A-619 011404A-620 Analyte Found (ppt) = (peak area - intercept) / slope x DF f i Recovery (%) - [analyte found (ppt)-analyte found in control (ppt)l x 100 amount added (ppt) Std. Cone. (ppt) 0 25 50 100 250 500 1000 - _ 25 50 100 - - 250 500 1000 Dilution Factor '1 1 1 - - 100000 10000 10000 - - - Peak Area 1666 12558 23706 41771 103160 203744 390620 2571 877 22595 202320 12239 22625 40020 19875 72159 69726 99551 199102 383257 Analyte Found Amount Added Analyte Recovery Found (ppo (ppo (%) (PPb) -- -- -- -- -- -- -- -- -- -- -- -- '- - -- -ND . ._ 50.4 50 101 - 513 500 103 -- -- -- -- -- -- 4340000 2500000 102 - 1780000 - - 14200 1720000 - - 13800 -- -- -- -- -- -- Standard Curve : Linear (1/x weighted) Intercept =: 3007.38 Slope = 388.640 Coef. Of Det. = 0.999379 Total Solids (%) - _ 48.73 48.73 - Analyte Found (ppb) = [analyte found (ppt) x volume extracted (0.04 L)] / sample weight (5 g) t Analyte Found (ppb) dry weight = analyte found (ppb) x (100% / total solids (%)) CS = Calibration standard C - Control sample C ; S = Sample LF = Lab fortified sample FF = Field fortified sample LCS = Laboratory Control Spike CK - Check Standard ND = Not detected = Response between 0 arid 25 ppt NQ = Not quantifiable = Response between 25 ppt and LOQ (50 ppt) Spreadsheet prepared by: Analyte Found (ppb) Dry Weight - - 29100 28300 - 000386 ft 358 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 Internal Chain of Custody/Fortification Sheet Exygen Study Number: L1445 Matrix: Sludge Sponsor Study/Protocol No: NA The samples listed below were removed from refrigerator No. * * Time Q&OO Date A l | H '\0 14 Initials. CLIENT SAMPLE ID na na na D A I-121003-N W -02 D A I-121003-N W -02 D A I-121003-N W -02 EXYGEN ID NUMBER Reagent Blank Reagent Spk A Reagent Spk B L1445-2 Spk C L1445-2 L1445-2 Rep _ W EIGHT (g) _ _ _ 5.0 5.0 5.0 _ FORTIFICATION (ng) _ 2.0 20.0 100000.0 _ _ _ f. 1i _ _ - __ _ __ _ _- _ - __ _ _ __ - _- _ - __ _ _ _- _ _ -_ - _- - - -_ - - -- : : Spiking Solution Used Volume Used for Spiking Initial/Date Reagent Spk A F120903-5 (10 ng/mL) 200 pL (200 pL micropipet) tiff- /Ol Reagent Spk B F120903-4 (100 ng/mL) 200 pL (200 pL micropipet) W f /Ol 4 * - L1445-2 Spk C S120803-1 (1000000 ng/mL) 100 pL (200 pL micropipet) K l /M f. _ _ - - I? _ _ _ - _ _- _- All samples were weighed on balance No. 2 0 H' Time 0 ^ 3 0 Date Ol Initials - _ 3 2-After weighing samples were returned to refrigerator No. , Time 3 DO- D a te ___Q i Initials Analysis Summary: Data Set: o i i M o ^ A f Data Set:______~~ Data S et:_____ Set extraction/analysis data verified by: 0 / 7 ) f '' 1/ Initials/Date: Initials/Date: Initials/Date: -5f /__ Date: m u 1 " 1 .< > i ARCI :i:i :> ::r 3058 Research Drive Phone: 814-272-1039 State College, PA 16801 Fax: 814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: L1445 MATRIX: Sludge METHOD: ExM-023-014 $$ ANALYTES: PFOA PROTOCOL NUMBER: NA Client ID na na na DAI-121003-NW-02 DAI-121003-NW-02 DAI-121003-NW-02 _ _ _ _ _ _ _ - ExygenID Reagent Blank Reagent Spk A Reagent Spk B L1445-2 Spk C L1445-2 L1445-2 Rep - - - - - STEP STEP STEP 12 3 \ 1 1/ ----- --- -- --- ----- .1, / - -- - - - *Initials/Date _ 0 ,1 k 3 & a l & STEP 1: Add 5mL of methanol and shake by hand for ~1 minute STEP 2: Bring up to 40 mL with hypercarb filtered type I water STEP 3: Centrifuge for 10 minutes at -3000 rpm STEP 4: Filter through glass acrodisc STEP 5: SPE column clean up STEP 6: Final volume to 5 mL collected in 15 mL polypropolene tubes STEP 7: LC/MS/MS analysis STEP 8: LC/MS/MS reanalysis. STEP 4 / \1 - - - di & STEP 5 \ / 1 - - - - - - - - - - 7/ J 61 i<u STEP 6 Dilutions (mL/mL) -- - STEP 7 I 1 \ y y x o ___ N --- --- --- -- -- -- -- ---- -- ----- a B p f C>1 Dilutions (mL/mL) - - - - - - STEP 8 -- - - - - - -- Reagents/ Materials Methanol C18 SPE Type I Water - Lot# NA - -- ---- - Initials/Date - 1-, -, R io i m o- (/ l 1 -- - -- -- HPLC Methanol H3S34S Ammonium Acetate Type water NA - - jL* Initials/Date oi 1)5 W *Initials and date under each step indicates the personnel that performed this step. $$ Method of Analysis for the Determination of Perfluorooctanesulfonate (PFOS) and Pentadecafluorooctanoic Acid (PFOA) in Soil _ COMMENTS: Final extracts stored in refrigerator J ^""Initials: Date: bli i July 19,2001/4 000388 :::n '"T? '1 > i RESEARC 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 Protocol No.: Method No.: PREPARATION OF EXTRACTED CALIBRATION STANDARDS None 01M-008-046* Exygen Study No.: NA Analytes: PFQA Matrix: Sample Vol: Exygen study n o . Tvne I WaterA 40 mT. Sponsor Sample ID NA NA NA NA NA NA NA NA Exygen Sample ID 0106020 0106020 0106020 0106020 0106020 0106020 0106020 0106020 - Sample Description Fort. Solution ID Type I WaterA - TypeIW aterA F120903-5 Type I WaterA F120903-5 Type I Water'' Type I WaterA F120903-5 F120903-4 Type I WaterA Type I WaterA F120903-4 F120903-4 Type I WaterA - F102703-2 - Fort. Fort. Soin. Cone. Volume (ng/mL) - ... (ml) - Micropipet used (uL) _ 10 100 200 10 200 200 10 400 200 100 100 200 100 200 200 100 400 200 100 100 200 - -.- Fort. Level (ppt) 25 50 100 250 500 1000 250 Final Solution ID #** X C 0 1 1404-0 X C 0 1 1404-1 XC011404-2 XC011404-3 X C 0 1 1404-4 X C 0 1 1404-5 X C 0 1 1404-6 XC011404-7 - Reagents/ ' Materials Methanol C18 SPE Type I Water LOt# fyi3l)2-"2>\ NA Initials/Date: Ctf **This must be a unique number. Use this system: Extracted Calibration Soln ID#: XCMMDDYY-0,1,2,3. etc. Samples removed froiyreirigeratd$/ freezer # 32- Time: OfiOQ Initials/Date: Ci l\jlH\&5cr\> 40 mL of each sample measured using a mT. graduated cylinder. After measuring, samples returned ttfrefrigeratpr / freezer # 3 2 - Time- jLjQO Samples fortified: SPE clean-up: Initials/Date: c t L / Initials/Date: Ctf 'c r s ' !/ .\ . mi |i--/ Initials/Date: (& /iwjSr`{ IH \i&tH THIS IS AN EXACTCOPY OF THEoriginal document. BY----- fU, L daT E ^ O lllljo ^ Final volume adjusted to 5 mL: Initials/Date: CEE /Qij^H Extracts placed in refrigerator # Initials/Date: CEE / Di ' STANDARD EXPIRATION DATE: 1/28/04 Comments: AThis type I water has been filtered through a hypercarb filter * Method of Analysis for the Determination of Ammonium Perfluorooctanoate (APFO) in Water. Vjd C E E Otj|4\^ July 10,2001/0 000389 Tr? '1 1 ' z ) :~~Z3. : m Masslynx - Sample List Sample List: C:\MASSLYNX\Fluoroche Qlcals.PRO\SampleDB\011404A Daikin Soil.SPL Printed: Thu Jan 15 13:30:31 2004 L ________________________________ Exygen study NO, M M 4 5 Page 1 Page Position: (1,1) Vial File Name LIMS ID Client ID Sample Description 1 11 011404A-601 ___ 2 12 011404A-602 -- 3 13 011404A-603 -- 4 14 011404A-604 -- 5 15 011404A-605 -- 6 16 011404A-606 -- 7 17 011404A-607 -- 8 92 011404A-608 -- 9 21 011404A-609 -- 10 22 011404A-610 -- 11 23 011404A-611 -- 12 12 011404A-612 -- 13 13 011404A-613 -- 14 14 011404A-614 -- 15 24 011404A-615 -- 16 25 011404A-616 -- 17 26 011404A-617 -- 18 15 011404A-618 -- 19 16 011404A-619 -- 20 17 011404A-620 -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- XC011404-0, 0 ng/L standard XC011404-1,25 ng/L standard XC011404-2,50 ng/L standard XC011404-3,100 ng/L standard X C011404-4, 250 ng/L standard XC011404-5, 500 ng/L standard XC011404-6,1000 ng/L standard Methanol Wash Reagent Blank Reagent Spk A, 50 ng/L Reagent Spk B, 500 ng/L X C011404-1,25 ng/L standard XC011404-2, 50 ng/L standard XC011404-3,100 ng/L standard L1445-2 Spk C, 2500000 ng/L, D F L1445-2, DF=10000 L1445-2 Rep, DF=10000 XC123003-4, 250 ng/L standard XC123003-5, 500 ng/L standard XC123003-6,1000 ng/L standard Matrix Sample Type Cone (ng/L) Cone B Cone C Test ID DF -- Blank -- Standard ___ Standard ___ Standard ___ Standard __ Standard -- Standard -- Blank ___ Blank ___ QC -- QC -- Standard ___ Standard ___ Standard __ QC ___ Analyte -- Analyte ___ Standard ___ Standard -- Standard 0 25 50 100 250 500 1000 -- -- 50 500 25 50 100 2500000 -- -- 250 500 1000 ___ -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- 01 01 01 01 01 01 01 01 01 01 01 01 01 01 0 100000 0 10000 0 10000 01 01 01 000390 11 Masslynx - Sample List Sample List: C:\MASSLYNX\Fluorochemie iJls.PRO\SampleDB\011404A Daikin Soil.SPL Printed: Thu Jan 15 13:30:31 2004 qiIis K ------------------------------ MS Method HPLC Method MS Tune File Inj.Volume 1 PFOA Fluorochems Fluorochems 15 2 PFOA Fluorochems Fluorochems 15 3 PFOA Fluorochems Fluorochems 15 4 PFOA Fluorochems Fluorochems 15 5 PFOA Fluorochems Fluorochems 15 6 PFOA Fluorochems Fluorochems 15 7 PFOA Fluorochems Fluorochems 15 8 PFOA Fluorochems Fluorochems 15 9 PFOA Fluorochems Fluorochems 15 10 PFOA Fluorochems Fluorochems 15 11 PFOA Fluorochems Fluorochems 15 12 PFOA Fluorochems Fluorochems 15 13 PFOA Fluorochems Fluorochems 15 14 PFOA Fluorochems Fluorochems 15 15 PFOA Fluorochems Fluorochems 15 16 PFOA Fluorochems Fluorochems 15 17 PFOA Fluorochems Fluorochems 15 18 PFOA Fluorochems Fluorochems 15 19 PFOA Fluorochems Fluorochems 15 20 PFOA Fluorochems Fluorochems 15 000391 it :::Tn T 3 : : ' i Exygen STUDY NO :3 " : i Page 2 Page Position: (2,1) IJ LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: N A t! Exygen Study No: L I445 Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #6) &' Computer: COMPAQ Professional Workstation AP200 r^ Software: Microsoft Windows NT: Version 4 Build 1381 : Service Pack 5 i . Micromass Limited: MassLynx 3.4 Build 004 HPLC Equipment: Hew lett Packard (HP) Series 1100 n HP Bin Pump HP Vacuum Degasser HP Autosampler H P Column Oven HPLC Column: Genesis C-8, 5 cm x 2.1 m m i.d. x 4 p (Exygen ID: 74A) (JONESCHROMATOGRAPHY: Part No. FK5962E) Mobile Phase (A) : Mobile Phase (B) : Analyst: 2 mM Ammonium Acetate in Type I Water Methanol Karen Risha Exygen Research 3058 Research Drive, State College, PA 16801 Phone: (814) 272-1039 FAX: (814) 231-1580 O' b \' 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:_____ ^ ________ n I) n n 000392 Scanning Method Report Method: C :\MASSLYNX\FLUOROCHEMICALS .PRO\ACQtJDB\PFOA Last Modified: Wed Mar 26 15:31:10 2003 Printed: Thu Jan 15 13:34:17 2004 Solvent Delay ( mins ) : 0.00 Analog Channel 4 : Unused Function : 1 MRM of 1 Mass Pair ( ESP- ) Inter Channel Delay ( Secs ) : Span ( Daltons ) : Start Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 8.00 1 Dwell (Secs) Coll Energy (eV) Cone ( V ) 1 413.00 369.00 0.20 10 10 Page 1 000393 &1 t- ! Method Report Method File: mF : Last Modified: c:\masslynx\fluorochernicals.pro\acqudb\fluorochems Thursday, January 15, 2004 13:34:23 Page 1 A% n B% !; ] c% ' ' D% 60.0 40.0 o.o 0.0 p Flow (ml/min) ' Stop Time (mins) 1 Min Pressure (bar) Max Pressure (bar) 0-- , Oven Temperature Left(C) f ; Oven Temperature Right(C) 0.300 14.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable ; : The gradient I- : Time 0.00 0.40 1.00 7.00 7.50 9.00 i. 9.50 13.50 14.00 Timetable A% 60.0 60.0 10.0 10.0 0.0 0.0 60.0 60.0 60.0 contains 9 entries which are - B% 40.0 40.0 90.0 90.0 100.0 C% 0.0 0.0 0.0 0.0 0.0 100.0 40.0 0.0 0.0 40.0 0.0 40.0 0.0 : D% 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 6 entries which are : Time Column Switch Contactl - Contact2 Initial Off Off Off 0.00 Off On Off 0.05 Off Off Off ( 0.10 7.95 Off Off On Off Off Off 8.00 Off Off Off Contact3 Off Off Off Off On Off HP1100 Autosampler Initial Conditions Draw Speed * ; Eject Speed (/l/min) Draw Position (mm) Stop Time (mins) Injection Volume ( f i l ) T u Vial Number 200.0 200 0.50 14.00 15.0 17 b' Flow 0.300 0.300 0.300 0.300 0.300 0.400 0.400 0.400 0.300 Contact4 Off Off Off Off Off Off Pressure 400 400 400 400 400 400 400 400 400 p r~r 0 0 0 3 9 4 ir ! (a. : ? Tuning Method Report r-f Method: ri Printed: H t; C :\MASSLYNX\FLUOROCHEMICALS .PRO\ACQUDB\FLUOROCHEMS Thu Jan 15 13:34:38 2004 ' .Dlpp-f n n Page 1 * n H- n SOURCE ( ESP- ) g.- Capillary Cone p Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. n Desolvation Temp. i Pressures Analyser Vacuum Gas Cell f: in / --i Set Rdbk 3.00 20 0.0 0.0 0.0 100 300 -2.93 -36 100 299 Rdbk OFF 3.0e-3 Analyser LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas Flows Cone Gas Desolvation Set Rdbk 14.0 14.0 1.0 -2 15 2 14.0 14.0 2.0 650 37 39 41 -648 Rdbk 132.9 761.5 000395 Quantify Calibration Report Study No.:Ll445, Set No.:011404A, Ext.Date:01/14/04, Analyst:K.Risha Page 1 Calibration: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\CurveDB\011404A Daikin Soil M Last modified: Fri Jan 16 09:23:57 2004 Printed: Fri Jan 16 09:25:14 2004 Exygen Research, 3058 Research Drive, State College, PA 16801 000396 Quantify Sample Report Study No.:L1445, Set No.:011404A, Ext.Date:01/14/04, Analyst:K.Risha Page 1 Sample List: Last modified: Method: Last modified: Job Code: Printed: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\011404A Daikin Fri Jan 16 09:18:46 2004 P:\Data\LCMSMS6 \Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Tue Jan 13 07:47:06 2004 ,1a Fri Jan 16 09:25:15 2004 Initials - Date Run# jQ l A E S -)t)| to h m t M k ' L i o Soil Name: 011404A-601 Text: 1: C8 Acid Exygen Research, 3058 Research Drive, State College, PA 16801 000397 Quantify Sample Report Study No.:L1445, Set NO.:011404A, Ext.Date:01/14/04, Analyst:K.Risha Page 2 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\011404A Daikin Soil Last modified: Fri Jan 16 09:18:46 2004 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 Job Code: Printed: Fri Jan 16 09:25:15 2004 Name: 011404A-602 Text: 1: C8 Acid Exygen Research 3058 Research Drive, State College, PA 16801 000398 H : Quantify Sanale Report Study N o .:Iil445, Set No.:011404A, Ext.Date:01/14/04, Analyst :K.Ri sha ' Page 3 F-y Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\011404A Daikin Soil fe i Last modified: Fri Jan 16 09:18:46 2004 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 n Job Code : Printed: Fri Jan 16 09:25:15 2004* * Name: 011404A-603 Text : 1 : C8 Acid ni- < rn ITS f- Exygen Research, 3058 Research Drive, State College, PA 16801 000399 M- Quantify Sample Report Study No.:L1445, Set No.:011404A, Ext.Date:01/14/04, Analyst:K.Risha Page 4 rr Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\011404A Daikin Soil * Last modified: Fri Jan 16 09:18:46 2004 Method: P:\Data\LCMSMS6 \Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 f~i Job Code: Vk >( Printed: Fri Jan 16 09:25:15 2004 Name: 011404A-604 Text: 1: C8 Acid XC011404-3,100 ng/L standard 0 1 1404A-604 Sm (Mn, 2x2) 100n %: 5.37 15-Jan-2004 22:57:28 LC/MS/MS #6 MRM of 1 Channel ES413 > 3 6 9 2 .0 6 e 5 Area n 0 - Lf = ?=T_l ' I i - -- r f T ^ F T T r P F r ' ' ! ...n < "i | ' r 1 T "| 1f i 1.00 2 .0 0 3.00 m f k 1 I1 f 4.00 i - i - p r - r - l ...l- 'i I I I I I , 5 .0 0 6.00 7.00 Tim e 8.00 t K H n Exygen Research, 3058 Research Drive, State College, PA 16801 000400 Quantify Sample Report Study No.:L1445, Set No.:011404A, Ext.Date:01/14/04, Analyst:K.Risha Rage 5 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\011404A Daikin Soil Last modified: Fri Jan 16 09:18:46 2004 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0A 010504 Last modified: Tue Jan 13 07:47:06 2004 Job Code: Printed: Fri Jan 16 09:25:15 2004 Mame: 011404A-605 Text: 1: C8 Acid XC011404-4, 250 ng/L standard 0 1 1404A -605 Sm (Mn, 2x2) 100i %: 15-Jan-2004 23:13:12 LC/MS/MS #6 5.36 MRM of 1 Channel ES413 >369 6.55e5 Area 0 CT I V I I I I I |r i --r " l -I I I I I I 'J I I I I I I ' I ' M ' I I 1.00 2.00 3.00 r' i "it 4.00 i1 " r~r^ 5.00 6.00 j- i- --........................i j T im e 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 000401 I) * ; Quantify Sample Report ' '- ' Study No.:L1445, Set No.:011404A, Ext.Date:01/14/04, Analyst:K.Risha Page 6 m Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\011404A Daikin Soil | ) Last modified: Fri Jan 16 09:18:46 2004 Method: P:\Data\LCMSMS6 \Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 r ) Job Code: I" ' ' Printed: Fri Jan 16 09:25:15 2004 ) Name: 011404A-606 Text : 1 : C 8 Acid - XC011404-5, 500 ng/L standard t 0 1 1404A-606 Sm (Mn, 2x2) I1 100-1 r- %: 5.36 2 0 3 7 4 4 "! A 1 15-Jan-2004 23:28:49 LC/MS/MS #6 M R M of 1 Channel ES413 >369 1.20e6 Area p Ii o: r " i 1 1 I T-- Ir -f" " i |p"i 1 1 11 r 1 1 1I I I r 1I I H "t I -rirI"r,T l ,iT , i'" TH- i - ii i rt ii il il fpi I''-'"I ti-1 p' i..111 I , 1 1 ' I 1 ' `.!' ' ' ``"~nr^Tr'-1T-r-Ir-i '. ,-'r Ii 1i 1i 1; 1i Ii 'i i1 1i 'i Ii TIim e 1.00 2 .0 0 3.00 4.00 5 .0 0 ________ 6 ,0 0 ________ 7T)0________ 8 .0 0 pi t h* Jf,cJ5 n t Exygen Research, 3058 Research Drive, State College, PA 16801 000402 ri n r : Quantify Sample Report Study No.:L1445, Set No.:011404A, E x t .Date:01/14/04, Analyst:K.Risha Page 7 n Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\011404A Daikin Soil I < Last modified: Fri Jan 16 09:18:46 2004 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0A 010504 Last modified: Tue Jan 13 07:47:06 2004 i Job Code: li ' ' ' Printed: Fri Jan 16 09:25:15 2004 Name: 011404A-607 Text: P 1: C8 Acid XC011404-6,1000 ng/L standard 0 1 1404A -607 Sm (Mn, 2x2) f; 100n *i si %: E OQ 3906201 I 1 15-Jan-2004 23:44:34 LC/MS/MS #6 M R M of 1 Channel ES413 > 3 6 9 2.26e6 Area tn\ 0 J ir"T"ii i i i i i i i i r i t"H" i \ t i f"\") rn-- i-- i-- | t !-- i ! | rn ; i'i"T'i rr]"i.p-7i,i-i_ij-- 11 7-' '-i-| i ' i-TY i t i - i i T im e 1.00 2.00 3.00 4 .0 0 ________ 5 ,0 0 ________ 6X)0________ 7TX)________8 .0 0 r~, ti t- \ n n n f ?: tn n Exygen Research, 3058 Research Drive, State College, PA 16801 000403 n . ............. f ; Quantify Sample Report '- Study No.:L1445, Set No. :011404A, Ext .Date: 01/14/04, Analyst :K.Risha Page 8 P Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\011404A Daikin Soil | Last modified: Fri Jan 16 09:18:46 2004 Method: P:\Data\LCMSMS6 \Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 i Job Code: f; ' ; ., '' '' ' Printed: Fri Jan 16 09:25:15 2004 i ; Name: 011404A-608 Text: n I k' \> n Exygen Research, 3058 Research Drive, State College, PA 16801 000404 n pI*- ( Quantify Sample Report Study No.:L1445, Set No.:011404A, Ext.Date:01/14/04, Analyst:K.Risha Page 9 Sandle List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\011404A Daikin Soil i Last modified: Fri Jan 16 09:18:46 2004 Method: ; P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0A 010504 Last modified: Tue Jan 13 07:47:06 2004 p Job Code: ft - . Printed: Fri Jan 16 09:25:15 2004 ` Name: 011404A-609 Text: It ! jk 4 H i i' flt n n Exygen Research, 3058 Research Drive, State College, PA 16801 bt . 000405 Quantify Sample Report Study No.:L1445, Set No.:011404A, Ext.Date:01/14/04, Analyst:K.Risha Page 10 r- Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\011404A Daikin Soil i Last modified: Fri Jan 16 09:18:46 2004 1 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0A 010504 Last modified: Tue Jan 13 07:47:06 2004 H Job Code: : Printed: Fri Jan 16 09:25:15 2004 6 Name: 011404A-610 Text : l* nJk s - 1> n p n !: n f Exygen Research, 3058 Research Drive, State College, PA 16801 p? 000406 t Quantify Sample Report * Study No.:L1445, Set No.:011404A, Ext.Date:01/14/04, AnalystsK.Risha Page 11 f! Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\011404A Daikin Soil I Last modified: Fri Jan 16 09:18:46 2004 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 Job Code: Printed: Fri Jan 16 09:25:15 2004 n I Name: 011404A-611 Text : f: r- F r~. Exygen Research, 3058 Research Drive, State College, PA 16801 000407 fr [ , Quantify Sample Report 1 Study No.:L1445, Set No.:011404A, Ext.Date:01/14/04, Analyst:K.Risha Page 12 r* Sample List: P :\Data\LCMSMS6 \Masslynx\Fluorochemicals.PRO\SampleDB\011404A Daikin Soil ITi Last modified: Fri Jan 16 09:18:46 2004 1 Method: P:\Data\LCMSMS6 \Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 f"1 Job Code: Printed: Fri Jan 16 09:25:15 2004 r Name: 011404A-612 Text : \! t; n t; fj n ) H n * Exygen Research, 3058 Research Drive, State College, PA 16801 000408 I * Quantify Sample Report ' Study No.:L1445, Set No.:0li404A, Ext.Date:01/14/04, Analyst:K.Risha Page 13 fi Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\011404A Daikin Soil | Last modified: Fri Jan 16 09:18:46 2004 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 r" Job Code: Ju ' - ' '' Printed: Fri Jan 16 09:25:15 2004 Name: 011404A-613 Text: pi f1 n I Exygen Research, 3058 Research Drive, State College, PA 16801 000409 Ii : ; Quantify Sample Report Study No.:Ll445, Set No.:011404A, Ext.Date:01/14/04, Analyst:K.Risha Page 14 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\011404A Daikin Soil | ; Last modified: Fri Jan 16 09:18:46 2004 ' Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 f*' Job C ode: ii , , .. . Printed: Fri Jan 16 09:25:15 2004 Name: 011404A-614 Text: .1: C8 Acid XC011404-3,100 ng/L standard 0 1 1404A-614 Sm (Mn, 2x2) 100n % :fc- - j 16-Jan-2004 01:34:12 LC/MS/MS #6 5.41 MRM of 1 Channel ES4 1 3 > 369 1,88e5 Area f"5 l- f=i= 1 1 I 1 !"' ^~r ^ T n ~r i T T~r?^r%i T im e 1.00 2.00 3 .00 4.00 5.00 6.00 7.00 8.00 in f n n t i- ! I3 Exygen Research, 3058 Research Drive, State College, PA 16801 n 000410 ; Quantify Sample Report ' Study No.:L1445, Set No.:011404A, Ext.Date:01/14/04, Analyst:K.Risha Page 15 mm Sanale List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\011404A Daikin Soil jf ' Last modified: Fri Jan 16 09:18:46 2004 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 p* Job Code : l-i ' * ` Prxnted: ' Frx Jan 16 09:25:15 2004 '' Name: 011404A-615 Text: is i t t L,, ? ' t ' n Exygen Research, 3058 Research Drive, State College, PA 16801 000411 1*1 f i Quantify Sample Report r j Study No.:L1445, Set No.:011404A, Ext.Date:01/14/04, Analyst:K.Risha Page 16 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\011404A Daikin Soil Last modified: Fri Jan 16 09:18:46 2004 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0A 010504 Last modified: Tue Jan 13 07:47:06 2004 f] job Code : f! Printed: Fri Jan 16 09:25:15 2004 Name: 011404A-616 Text : t* P tb i. P 1= t1 n t. ' p t Exygen Research, 3058 Research Drive, State College, PA 16801 000412 Quantify Sample Report Study No.:Iil445, Set No.:011404A, Ext.Date:01/14/04, Analyst:K.Risha Page 17 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\011404A Daikin Soil Last modified: Fri Jan 16 09:18:46 2004 Method: P:\Data\LCMSMS6 \Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 Job Code: Printed: Fri Jan 16 09:25:15 2004 5^ T- _J o '- Name: 011404A-617 Tent: 1: C8 Acid 5-2 Rep, DF=10000 34A-617 Sm (Mn, 2x2) 16-Jan-2004 02:21:13 LC/MS/MS #6 5.37 MRM of 1 Channel ES413 >369 3.20e5 Area o'' ' ' c U 1 1 11 11 1 1 '"1 1 f'7T J 1'i "~T", 1I i ! 1 1 11 1 1 ' 1.00 ' 2.00 3.00 4.00 5.00 6.00 7 .0 0 8.00 Escygen Research, 3058 Research Drive, State College, PA 16801 000413 Quantify Sample Report Study No.:L1445, Set No.:011404A, Ext.Date:01/14/04, Analyst:K.Risha Page 18 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PRO\SampleDB\011404A Daikin Soil J' Last modified: Fri Jan 16 09:18:46 2004 Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0A 010504 Last modified: Tue Jan 13 07:47:06 2004 Job Code: Printed: Fri Jan 16 09:25:15 2004 Name: 011404A-618 Text : t .. nI.< ! r*> Exygen Research, 3058 Research Drive, State College, PA 16801 000414 Hi : Quantify Sample Report Study No.:Ll445, Set No.:011404A, Ext.Date:01/14/04, Analyst:K.Risha Page 19 Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\011404A Daikin Soil ... Last modified: Fri Jan 16 09:18:46 2004 fe ji Method: P:\Data\LCMSMS6 \Masslynx\Fluorochemicals.PRO\MethDB\PFOA 010504 Last modified: Tue Jan 13 07:47:06 2004 Job Code: f- < fcw Printed: Fri Jan 16 09:25:15 2004 i Name: 011404A-619 Text : n 1: C8 Acid XC123003-5, 500 ng/L standard 0 1 1404A -619 Sm (Mn, 2x2) - -- t1 V 10O 1 - %- 5.40 199102 16-Jan-2004 02:52:35 LC/MS/MS #6 M RM of 1 Channel ES413 > 369 1 .1 3 e 6 Area n 1 - 1.00 2.00 3.00 '`T"r~l' 4 .0 0 5.00 6.00 7 .0 0 ' ! I T im e 8.00 fl *; f W *1 n -i fei -J Exygen Research, 3058 Research Drive, State College, PA 16801 000415 !**!! < Quantify Sample Report - li Study No.:L1445, Set No.:011404A, Ext.Date:01/14/04, Analyst:K.Risha Page 20 r"< Sample List: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\SampleDB\011404A Daikin Soil ! Last modified: Fri Jan 16 09:18:46 2004 1 J Method: P:\Data\LCMSMS6\Masslynx\Fluorochemicals.PR0\MethDB\PF0A 010504 Last modified: Tue Jan 13 07:47:06 2004 r* Job Code: I: 1 ' Printed: Fri Jan 16 09:25:15 2004 [ Name: 011404A-620 * ' Text : t K i' tL J r* H LJ * -I l Exygen Research, 3058 Research Drive, State College, PA 16801 000416 yr^TOfiV*^. g p " V ^ rrrflr*ij Date: 1-07-04 J x_yyn 1 xSbcJCh 1 J 1 1 1 3 T ^3 Analyst Initials Date and Time Data Aquired (ctrl+t) I sha I shz 07-Jan-04 13:52 | 07-Jan-04 13:52 shz 08-Jan-0413:08 I | Exygen ID L0001445-0002 CLIENT ID MATRIX PAN ID PAN WEIGHT (g) SAMPLE +PAN (g) DRIED SAMPLE +PA N (g) % Solids MOISTURE | SOLID 15 1.2825 21.1781 10.9775 48.7294 y' y y ''" y' ' ay' y' y' y' y^ / y^ y' / /U 'V 'y Vy^ y 000417 %solid L1445 Page 1 Date: 1-07-04 W l" xyn ^sS cFF1 ? Item Sample Sample Sample Sample Comment About 20 g of sample was weighed in aluminum weighing dishes using balance 9 (IN0000288) .shz 1-07-04 sample was placed into oven 2 (IN0000062) at 104C for over night time in 1355 temp in 104C .shz 1-07-04 Sample was removed from oven time out 1255 temp out 104C and cool in desiccator 6 (IN160) .shz 1-08-04 Weighed sample using balance 9 (IN0000288).shz 1-08-04 000418 %solid L1445 Page 1
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