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AR226-3587 P -2 Proven Results. 06 FE3 - ' rt r Analytical Report Fluorochemical Characterization of Aqueous Samples Fayetteville C8 Sampling 11/05 Exygen Research Laboratory Report No. L0006767 (Amended Final Report) Testing Laboratory Exygen Research 3058 Research Drive State College, PA 16801 Requester Michael D. Aucoin URS Corporation Barley Mill Plaza Bldg 19 Room 2118 Lancaster Pike and Rt 141 Wilmington, DE 19805 PAGE 1 0 F 5 058 Research Drive \State College, PA 16801, USA J : 800.281.3219 F: 814.272.1019 exygen.com P-3 1 Introduction Results are reported for the analysis of water samples received by Centre Analytical Laboratories, Inc. (dba Exygen Research) (Exygen) from DuPont Corporation. This report presents results assigned to Exygen Research study number L0006767. This report Is an amended report of Exygen Research study number L0006767. This amended report utilizes a different technique for determining signal to noise ratios for the determination of limit of detection and limit of quantification than in the original report. Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC/MS/MS) was requested for all samples. A total of 3 samples were received for analysis. The sample was prepared and analyzed by LC/MS/MS for the following list of fluorochemicals: Table 1: Target Analysis Comoound Name Ammonium Perfluorooctanoate Perfiuorooctanoic Acid Acronym APFO PFOA 2 Sample Receipt The samples were submitted in plastic containers, cooled with wet ice. The samples were collected on 11/16/05 and were received on 11/17/05. Chain-of-custody information is presented in Attachment C. 3 Holding Times The analytical method used was validated against a maximum holding time of 14 days in water samples. All samples were analyzed within the required holding time. 4 Methods - Analytical and Preparatory 4.1 LC/MS/MS 4.1.1 Sample Preparation for LC/MS/MS Analysis Water samples were initially treated with 200 uL of 250 mg/mL sodium thiosulfate solution to remove residual chlorine. Solid phase extraction (SPE) was used to prepare the samples for LC/MS/MS analysis. A forty-milliliter portion of sample was transferred to a C 18 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. PAGE 2 OFS P-4 4.1.2 Sample Analysis by LC/MS/MS A Hewlett-Packard HP1100 HPLC system coupled to a Micromass Ultima MS/MS was used to analyze the sample extracts. Analysis was performed using selected reaction monitoring (SRM). Samples were extracted and analyzed on 11/18/05. Raw analytical data can be found in Attachment D. 5 Analysis 5.1 Calibration An 8-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 5, 10, 25, 50, 100, 250, 500, and 1000 ng/L (ppt), as perfluorooctanoic acid (PFOA). Th 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 ( r ) were determined. A calibration curve is acceptable if r > 0 992 ( r > 0.985). --' Calibration standards for MS/MS analysis were prepared using the same SPE procedure used for samples. For the results reported here, calibration criteria were met. 5.2 Blanks Extraction blanks were prepared and analyzed with every extraction batch of samples. The extraction blanks should not have any target analytes present at or above the limit of detection. 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 limit of detection. For the samples presented here the instrument blanks are compliant. 5.3 Surrogates Surrogate spikes are not a component of the LC/MS/MS analytical method. 5.4 Matrix Spikes A matrix spike was prepared for each field sample at 5000 ng/L. The matrix spike recovery was within the acceptable range of 70 - 130%. Matrix spike recoveries are qiven in Attachment B. 5.5 Duplicates Each field sample was analyzed in duplicate. Results are given along with the sample results in Attachment A. PAGE3 OF5 P-5 5.6 Laboratory Control Samples Milliq 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%. 5.7 Sample Related Comments A single analytical run was performed to complete the sample analysis. The following is a brief quality control narrative for the run. Analytical Samples Analyzed Run Number Comments 111805 A FAY-D-4328MLR, FAY-D-6999PED, All quality control results were FAY-K-FBLK-1 acceptable and all data are useable. 6 Data Summary Please see Attachment A for a detailed listing of the analytical results. All results are reported in (ng/L) parts per trillion as APFO and PFOA. 7 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. 8 Attachments 8.1 Attachment A: Results 8.2 Attachment B: Matrix Spike Recoveries 8.3 Attachment C: Chain of Custody 8.4 Attachment D: LC/MS/MS Raw Analytical Data 8.5 Attachment E: Standards Data PAGE 4 OF 5 Signatures PAGE5 OF5 p.7 > p.8 Analytical Report Analytical Results Fayetteville C8 Sampling 11/05 DuPont Sample Identification FAY-D-4328MLR FAY-D-4328MLR (laboratory duplicate) FAY-D-6999PED FAY-D-6999PED (laboratory duplicate) FAY-K-FBLK-1 APFO (ng/L) NQ NQ ND ND ND Limit o f Detection (LOD) for the procedure is approxim ately 4.5 ng/L Limit o f Quantitation (LOQ) fo r the procedure is 22 ng/L PFOA (ng/L) NQ NQ ND ND ND ND - Compound not detected NQ - Com pound detected at a level between the LOD and LOQ. Result is not quantifiable. ND < LOD < NQ < LOQ 0006 3058 Research Drive State College, PA 16801, USA VT: 800.281.3219 F: 814.272.1019 exygen.com Proven Results. P-9 Analytical Report Analytical Results Fayetteville C8 Sampling 11/05 DuPont Sample Identification FAY-D-4328MLR FAY-D-6999PED FAY-K-FBLK-1 APFO (ng/L) N N| TM Limit of Detection (LOD) for the procedure is approximately 4.5 ng/L Limit o f Quantitation (LOQ) for the procedure is 22 ng/L ND - Compound not detected PFOA (ng/L) NQ ND ND NQ - Com pound detected at a level between the LOD and LOQ. Result is not quantifiable. ND < LOD < NQ < LOQ Results are calculated according to the following criteria ! o D n f a 7 le l nd 'aob rat0ry duP|icate are greater than 5X LOQ, and the relative percent difference (KPU) is less than 20, the average value is reported: If the RPD is greater than 20 the hiaher value is reported. 'a If the sample and laboratory duplicate are less than 5X LOQ, and the absolute difference is less than rLoOnQnrttthHe average value is reported. If the absolute difference is greater than LOQ, the hi^gher value is 0007 3058 Research Drive vState College, PA 16801, USA T: 800.281.3219 F: 814.272.1019 exygen.com p. 10 Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: Spiked Amount (ng/L): FAY-D-4328MLR 5000 IPFOA Sample Concentration (ng/L) 9.95 Matrix Spike Result (ng/L) 5870 Matrix Spike Recovery (%) 117.2 Criteria (Pass / Fail) PASS Lower Recovery Limit: 70 Upper Recovery Limit: 130 Concentrations represent amount present as the PFOA anion Note: Sample results less than 13 ng/L are reported as NQ in the results section as they are below the limit of quantitation. Results are given in this table for recovery calculations only. 0008 Attachment B: LC/MS/MS Laboratory Spike Recovery Sample ID: | Spiked Amount (ng/L): | FAY-D-6999PED 5000 | |PFOA Sample Concentration (ng/L) 0 Matrix Spike Result (ng/L) 5250 Matrix Spike Recovery (%) 105.0 Lower Recovery Limit: 70 Upper Recovery Limit: 130 Concentrations represent amount present as the PFOA anion Criteria (Pass / Fail) PASS 0009 p. 13 3058 Research Drive RESEARCH State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 Project: P0000418 Company Name: DuPont Submitted By: Login Type: Started: Michael D. Aucoin Immediate Receipt of Samples True Date Start: Due Date: Received Date: Received By: 11/17/2005 11/27/2005 11/17/2005 Am merman, Mark Spread Sample: Label: Exygen SD/PI: Risha, Karen Project Title/Type: Analysis of Fluorochemicals in Water / ROUTINE Login Notes: Conform COC: Conform Sample: Conform Request: True True True Packaae ' K0007848 Carton Date / Condition Packages / Containers ShiDDer/ ID Received Date: 11/17/05 11:10 Package & Contents Uncompromised FEDEX 72742 6564 6567 Container # CO119853 C0119854 CO119855 CO119856 CO119857 CO119858 Gross Weiaht 562.80 g 551.20 g 540.90 g 549.00 g 574.40 g 585.80 g eM 8.40 8.20 4.70 4.40 9.70 9.80 Container TvDe 500 ml Clear Plastic Narrow 500 ml Clear Plastic Narrow 500 ml Clear Plastic Narrow 500 ml Clear Plastic Narrow 500 ml Clear Plastic Narrow 500 ml Clear Plastic Narrow Preservative NONE NONE NONE NONE NONE NONE TemD. Control/TemD. Wet Ice 0.8 Mfa. Lot Direction / Handled Bv RECEIVED Ammerman, Mark Mfa. ID SamDle ID L0006767-0001 L0006767-0002 L0006767-0003 Container C0119853 C0119854 C0119855 C0119856 C0119857 C0119858 Matrix LIQUID LIQUID LIQUID Fraction Water Samples Sample FAY-D-4328MLR Water FAY-D-6999PED Water FAY-K-FBLK-1 11/17/2005 Login.rpt 0010 Report Version: Aug 24 2005 3:47PM Page 1 of 2 Date Sampled 11/16/2005 Date Due 11/27/2005 11/16/2005 11/27/2005 11/16/2005 11/27/2005 instance: R0209072 R0209072 Login Reviewed By: Login p . 15 " f f y * ^ 7 7 / ^ ) y y \ _______________ Date/Time: / / / 'l l 0 ^ ^ 7S 11/17/2005 Login.rpt 0011 Report Version: Aug 24 2005 3:47PM Page 2 of 2 Instance: R0209072 lllllllll p. 16 PROJECT INFORMATION Client (name & address): AD-kh A? Srs.f*r- CHAIN OF CUSTODY/ANALYSIS REQUEST FORM Exygen Research Sample Receiving 3048 Research Drive State College, PA 16801, USA T: 8 1 4.231.8032 F: 814.2 3 1 .1 5 8 0 exygenresearch.com Page ANALYSES REQUESTED Project Managjer (Name &,lE-mail Address): f- j u fo f ^ _______________ Phone: Fax: Sampler: Project Name: RO Quotation # : ,,i , Please fill out this form completely to ensure correct analysis and proper handling of your samples. c. 'SOv \ rJ 'V. 's- SAMPLE ANALYSIS CHAIN OF CUSTODY Relinquished by -v? f4--h - Date Time ) 3 n OTHER INFORMATION Date Time ih il - o r U 2>0 <------- --- ------------ -- --------- " / '- j / i r - / / / o LAB USE ONLY PROJECT REQUIREMENTS Results Deadline: Laboratory Report Options: Sample results only CD Add case narrative CD Add quality control summary CD Add calibration summary CD Add raw data CD Other p . 17 ORIGIN ID: FAYA (910) 679-TT46 KEN '.CEADBETTER . - E I DUPONT/SIT SUPPORT 22828 NC HIGHWAY 87 W FAYETTEVILLE, NC 28306 > ( UNITED STATES US 'V " rofiTTN: SAMPLE'RECEIVING EXYGEGN RESEARCH 3048 RESEARCH DRIVE STAE COLLEGE, M 16501 ui ' Ship Dala : 16NOV05 Actual Ugt: 38.0 LB MAN -Systmll: 385790/CAFE2264 Account: S 028300174 ' Dimmed: 13x14x24 IN (814) 231-8032 FedEx Express wiiiiifiiiiaiiiiiKiuiiiiiu [)> 01 0216801 840 11 7242656465670201 DFelDiEvery02A8d3d0re0s1s74 320 1/1 38.0LB Y 3048 RESEARC Barcode BILL THIRD PARTY P R IO R IT Y OVERNIGHT TRK# 7242 6564 6567 0201 NV16801 -Pfl-us THU Deliver By: 17NOV05 SCPIET flflfl 31680124110000027242656465672016 i 0013 p. 18 Sponsor Study No: Exygen Study No: Analyte: Ions Monitored: Site: NA L6767 APFO 413->369 Fayetteville RAW DATA REPORT Limit of Quantitation (LOQ): Limit of Detection (LOD): Injection Volume: Matrix: Sample Volume: Final Volume: 22.4 ng/L 4.47 ng/L 15 pL Water 40.0 mL 5.0 mL Set No: Analyst: Instrument Type: Extraction Date: Analyzed on: III805A Karen Risha LC/MS/MS Unit # 7 11/18/05 11/18/05 Exygen ID X C110705-0 X C 110705-1 XC110705-2 XC 110705-3 XC110705-4 X C I10705-5 XC110705-6 XCI 10705-7 XCI 10705-8 XCI 10705-9 Methanol Wash Reagent Control L6767-3 Reagent Spk A Reagent Spk B L6767-1 SpkC L6767-2 Spk D Methanol Wash XCI 10705-1 XCI 10705-2 XCI 10705-3 XCI 10705-4 L6767-1 L6767-1 Rep L6767-2 L6767-2 Rep XCI 10705-5 XCI 10705-6 XCI 10705-7 XCI 10705-8 * Sponsor ID - . . . . . _ NA FAY-K-FBLK-l NA NA FAY-D-4328MLR FAY-D-6999PED . . _ _ FAY-D-4328MLR FAY-D-4328MLR FAY-D-6999PED FAY-D-6_999PED _ - Sample Code C CS cs cs cs cs cs cs cs CK C c s LCS LCS LF LF C cs cs cs cs s s s s cs cs cs cs Run No. I1I805A-100I 111805A-1002 111805A-I003 111805A-1004 111805A-1005 111805A- 006 111805A -1007 111805A -1008 111805A-1009 111805A-1010 111805A-1011 I11805A-I012 111805A-1013 111805A-I0I4 111805A-10I5 111805A-1016 1I1805A-1017 111805A-1018 111 805A -1019 111805A-1020 111805A-1021 111805A-1022 111805A-1023 111805A-1024 111805A-I025 111805A -1026 111805A-1027 111805A-1028 111805A-I029 111805A-1030 Std. Cone. (ng/L) 0 5 10 25 50 100 250 500 1000 250 - - - - - 5 10 25 50 - - - 100 250 500 1000 PFOA Found (ng/L) * (peak area intercept) / slope x DF Recovery (%) * [PFOA found (ngZL)-PFOA found in control (ng/L)l amount PFOA added (ng/L) x 100 Dilution Factor . . . , . . , . 1 1 1 1 10 10 . . . . . 1 1 1 1 . . - Peak Area 0 494 826 2065 3584 7752 16331 35308 69493 16694 0 73 0 4065 39560 41817 37432 0 410 807 1937 3814 832 917 0 0 7939 17931 35873 72903 APFO Found (ng/L) = PFOA found (ng/L) x (MW APFO (431)/ MW PFOA (414)) PFOA Found (ng/L) . APFO Found (ng/L) Amount PFOA Added . . ND ND 55.5 555 5870 5250 ND ND 57.8 578 6110 5470 50 500 5000 5000 . 9.95 NQ 11.1 NQ ND ND ND ND . . -- _ - Intercept : 125.839 Slope ' 70.9929 Coef. O f D et.a 0.998929 CS * Calibration standard C = Control sample S * Sample LF = Lab fortified sample FF * Field fortified sample LCS = Laboratory Control Spike Avg Resp. of the 250 ppt Standards (area): Response o f the Check Standard (area): Percent Difference (%): % difference acceptable if within 17131 16694 3 15% CK = Check Standard ND * Not detected * Response between 0 and LOD NQ Not quantifiable * Response between LOD and LOQ (>/,,) 111 111 117 105 - p. 20 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 Internal Chain of Custody/Fortiflcation Sheet Exygen Study Number: Sponsor Study/Protoco! No ^6767 NA Matrix: Water ~ The samples listed below were removed from refrigerator No. ^ 4 - Time ftf t Date CLIENT SAMPLE ID na na na FAY-D-4328MLR FAY-D-6999PED FAY-D-4328MLR FAY-D-4328MLR FAY-D-6999PED FAY-D-6999PED FAY-K-FBLK-1 - EXYGEN ID NUMBER Regent Control Reagent Spk A Reagent Spk B L6767-1 Spk C L6767-2 Spk D L6767-1 L6767-1 Rep L6767-2 L6767-2 Rep L6767-3 - - - VOLUME (mL) 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 40.0 _ FORTIFICATION (ng) 2.0 20.0 200.0 200.0 _. -- -- ---- -, - -_ -- -- - - - -' Reagent Spk A Reagent Spk B L6767-1 Spk C L6767-2 Spk D - ' All samples were measured: Time /: l>5 A m Spiking Solution Used F091305-5 (10 ng/mL) F091305-4 (100 ng/mL) F091305-3 (1000 ng/mL) F091305-3 (1000 ng/mL) - - - - Date J / h s b s p g Volume Used for Spiking 200 pL (200 pL micropipet) 200 pL (200 pL micropipet) 200 pL (200 uL micropipet) 200 pL (200 pL micropipet) _ . . . _ . - Initial/Date r t /li n< d F P /i,l,a htr / 'PfT /,,lip, /ill iA JOr - Initials j h - After measuring samples were returned to refrigerator No. & Time PM Date Initials <5Ob u ht/taA? Comments: 200 uL o f 250 mg/mL sodium thiosulfate was added to all samples before spiking. Initials/Date: ^ h / 1 Analysis Summary: Data Set: 1 I I 6 6 5 A Data Set Data Set -I-n-i-t-i-a-l-s-/-D- ate: 'Q1 J,.r /j M' I o s Initials/Date: -f-/ / Initials/Date: -- Set extraction/analysis data verified by: m L . 0015 m //A'~ r -- / Date: July 2C6, 2001/6 'c ^ r it h / W R ES EA RC H 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NUMBER: L6767 MATRIX: Water METHOD: QlM-QQ8-04frw ANALYTES: PFOA PROTOCOL NUMBER- NA Client ID na na na FA Y -D -4328M LR FAY-D-6999PED FA Y -D -4328M LR FA Y -D -4328M LR FAY-D-6999PED FAY-D-6999PED FAY-K-FBLK-l Exygen ID ReRent Control ReaRent Spk A ReaRent Spk B L6767-1 Spk C L6767-2 Spk D L6767-1 L6767-1 Rep L6767-2 L6767-2 Rep L6767-3 STEP 1 STEP 2 i-------- 1 V nI Dilutions (mL/mL) -- O '/l.D '/1 .0 -- -- -- STEP 3 Dilutions (mL/mL) STEP 4 X- / r-- - -- -- -- Reagents/ In itia ls/D a te Lot # or uA y^ui DL ft 'J7j 0e r/i/ .w<r ^ 0 IIIItIn * p. 21 0016 - - -- - --- - * * - " ''In itia ls/D a te - -- -- -- -- -- -- -- -- -- -- - tO O H u s 0 0 STEP 2. Final volume to 5 mL collected in 15 mL polypropolene tubes STEP 3: LC/MS/M S analysis STEP 4: LC/MS/MS reanalysis. ._ - __ - -_ - _. - w - .. - _. - __ __ -- In itia ls/D a te ^Initials and date under each step indicates the personnel that performed this step. $$ Method o f Analysis for the Determination o f Ammonium Perfluorooctanoate (APFO) in Water COMMENTS: Final extracts stored in refriRerator L Initials: D O Date: / / l l i l Z i ) o f V c n H x 'Z ' I f 1- -1 i f e July 12,2005/5 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 p. 22 0017 PREPARATION OF EXTRACTED CALIBRATION STANDARDS Protocol No.: None Method No.: 01M-008-046* Exygen Study No.: NA Analytes: PFOA Matrix: Wqfagteygen study n o . Uo7b1 Sample Vol: 40 mL Sponsor Sample ID Exygen Solution ID Sample Description Fort. Solution ID NA Water* - NA SLt>0lUo<i Water* F 0 9 1305-5 NA 3.LooILLf Water* F 0 9 1305-5 NA 5>oiLun Water* F 0 9 1305-5 NA Looaut Water* F 0 9 1305-5 NA 5LestlLLdJ Water* F 0 9 1305-5 NA SLoU a-i Water* F091305-4 NA SLOOILCI Water* F091305-4 NA SlQiacji-f Water* F091305-4 NA Water* F 0 9 1305-7 rerucai arrows in a column indicate identical values. Fort. Soin. Cone. __ing6nL) 10 10 10 10 10 100 100 100 ' 100 Fort. Volume (r L) 20 40 100 200 400 100 200 400 100 Micropipet used (PL) 20 200 200 200 200 200 200 200 200 Fort. Level (ddO 5 10 25 50 100 250 500 1000 250 Final Solution ID#** X C110705-0 X C 110705-1 XC 110705-2 X C110705-3 X C 1 10705-4 X C110705-5 X C 1 10705-6 X C110705-7 X C 1 10705-8 X C110705-9 Reagents/ Materials Lot it C 18SPE OMSJaMU Initials/Date: lUA-rln* **This must be a unique number. Use this system: Extracted Calibration Soln ID #: XCMMDDYY-0,1,2,3. etc Samples removed from ^frigeratjfr/ freezer # Time: V c o flm Initials/Date: 5 A / /lli'f/oS' 40 mL o f each sample measured usinga^ , S C mL graduated cy'li-n--d-e--r-. Initials/Date: Slif) After measuring, samples returned torfefiTgerator)/ f^re--e-z--e-r"it 3^P}__ T~ ime: 3 '- 3 b f ^ \ Initials/Date: </)A Samples fortified: Initials/Date: IW fe / j i l n i u r SPE clean-up: Initials/Date 6 / ul*7/oer Final volume adjusted to 5 mL: Initials/Date D D / lilo'floS Extracts placed in refrigerator # 32- Initials/Date ! / / h r f o s / I / I otIo* / i(l7o*f/ Tlii STANDARD EXPIRATION DATE: iib|c6 11/21/2005 Comments: AThis water has been filtered through a hypercarb filter Method of Analysis for the Determination of Ammonium Periluorooctanoate (APFO) in Water. July 12, 2005/1 Masslynx - Sample List Sample List: C:\MASSLYNX\008 APFC Printed: Fri Nov 18 12:55:12 2005 RO\SampleDB\111805A.SPL _______________ lx 0018 Vial File Name LIMS ID Client ID Sample Description Mai 1 1 111805A-1001 . . . ___ XC110705-0, 0 ng/L standard 2 2 111805A-1002 -- -- XC 110705-1, 5 ng/L standard 3 3 111805A-1003 -- -- X C 110705-2, 10 ng/L standard 4 4 111805A-1004 -- -- XC110705-3, 25 ng/L standard 5 5 111805A-1005 -- -- XC110705-4, 50 ng/L standard 6 6 111805A-1006 -- -- XC110705-5, 100 ng/L standard 7 7 111805A-1007 -- -- XC 110705-6, 250 ng/L standard 8 8 111805A-1008 -- -- XC 110705-7, 500 ng/L standard 9 9 111805A-1009 -- -- XC110705-8, 1000 ng/L standard 10 10 111805A-1010 -- -- XC110705-9, 250 ng/L check standard -- 11 92 111805A-1011 -- -- Methanol Wash 12 11 111B05A-1012 -- -- Reagent Control 13 12 111805A-1013 -- -- L6767-3 14 13 111805A-1Q14 -- Reagent Spk A, 50 ng/L 15 14 111805A-1015 -- -- Reagent Spk B, 500 ng/L 16 15 111805A-1016 -- -- - L6767-1 Spk C, 5000 ng/L, DF=10 17 16 111805A-1017 -- -- L6767-2 Spk D, 5000 ng/L, DF=10 18 92 111805A-1018 -- -- Methanol Wash -- 19 2 111805A-1019 -- -- XC110705-1, 5 ng/L standard 20 3 111805A-1020 -- -- XC 110705-2,10 ng/L standard 21 4 111805A-1021 -- -- XC 110705-3, 25 ng/L standard 22 5 111805A-1022 -- -- XC 110705-4, 50 ng/L standard 23 17 111805A-1023 -- -- L6767-1 24 18 111805A-1024 -- -- L6767-1 Rep 25 19 111805A-1025 -- -- L6767-2 26 20 111805A-1026 -- -- L6767-2 Rep 27 6 111805A-1027 -- -- XC110705-5, 100 ng/L standard 28 7 111805A-1028 -- -- XC110705-6, 250 ng/L standard 29 8 111805A-1029 -- -- XC110705-7, 500 ng/L standard 30 9 111805A-1030 -- ___ XC 110705-8,1000 ng/L standard Page 1 Page Position: (1,1) Sample Type Cone (ng/L) Cone B Cone C Test ID DF MS Method Blank Standard Standard Standard Standard Standard Standard Standard Standard QC Blank Blank Analyte QC QC QC QC Blank Standard Standard Standard Standard Analyte Analyte Analyte Analyte Standard Standard Standard Standard 0 5 10 25 50 100 250 500 1000 250 -- -- -- 50 500 5000 5000 -- 5 10 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 1 008 PFOA 0 1 008 PFOA 0 1 008 PFOA 0 1 008 PFOA 0 10 008 PFOA 0 10 008 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 1 008 PFOA 0 1 008 PFOA 0 1 008 PFOA p tCoJ Masslynx - Sample List Sample List: C:\MASSLYNX\008 APFOf>ROVSampleDB\111805A.SPL Printed: Fri Nov 18 12:55:12 2005 J j ) --------------------------- HPLC Method MS Tune File Inj Volume (pL) 1 water PFOA Tune 15 2 water PFOA Tune 15 3 water PFOA Tune 15 4 water PFOA Tune 15 5 water PFOA Tune 15 6 water PFOA Tune 15 7 water PFOA Tune 15 8 water PFOA Tune 15 9 water PFOA Tune 15 10 water PFOA Tune 15 11 water PFOA Tune 15 12 water PFOA Tune 15 13 water PFOA Tune 15 14 water PFOA Tune 15 15 water PFOA Tune 15 16 water PFOA Tune 15 17 water PFOA Tune 15 18 water PFOA Tune 15 19 water PFOA Tune 15 20 water PFOA Tune 15 21 water PFOA Tune 15 22 water PFOA Tune 15 23 water PFOA Tune 15 24 water PFOA Tune 15 25 water PFOA Tune 15 26 water PFOA Tune 15 27 water PFOA Tune 15 28 water PFOA Tune 15 29 water PFOA Tune 15 30 water PFOA Tune 15 jiO il Page 2 Page Position: (2, 1) p. 24 p . 25 Scanning Method Report Method: C:\MASSLYNX\008 APFO.PRO\ACQUDB\008 PFOA Last Modified: Wed Mar 20 15:07:50 2002 Printed: Fri Nov 18 13:17:55 2005 Solvent Delay ( mins ) : 0.00 Function : 1 MRM of 1 Mass Pair ( ESP- ) Inter Channel Delay ( Secs ) : Span ( Daltons ) : Start Time ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 8.00 1 Dwell (Secs) Coll Energy (eV) 1 413.00 369.00 0.20 10 Cone 10 Page 1 0021 Method Report Method File: Last Modified: Printed: c :\masslynx\008 apfo.pro\acqudb\water Friday, November 18, 2005 13:18:43 Friday, November 18, 2005 13:18:48 HP1100 LC Pump Initial Conditions Solvent s B% C% D% Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 50.0 40.0 0.0 0.0 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% 50.0 50.0 10.0 10.0 0. 0 0.0 50.0 50.0 60.0 50.0 B% 40.0 40.0 90.0 90.0 100.0 100.0 40.0 40.0 40.0 40.0 c% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 D% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 0.400 0.400 0.400 0.300 0.300 HP1100 LC Pump External Event Timetable The Timetable contains 4 entries which are : Time Initial 0.00 0.10 8 .00 Column Switch Off Off Off Off Contactl 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 (/il/rrtin) Draw Position (mm) Stop Time (mins) Injection Volume ( f i l ) Vial Number 200.0 200 0.10 15.00 15.0 9 p . 26 Pag Pressure 400 400 400 400 400 400 400 400 400 400 0022 Tuning Method Report Method: Pr;i-nted; C:\MASSLYNX\008 APFO.PRO\ACQUDB\PFOA TUNE Fri Nov 18 13:20:17 2005 I.OCIeCr - i -i .. 2 363.00 3 - - : ! ' 3 .- ";rf.- j i f f v r' J . ; ' ;:t: ;;: : :: . ; :4 ; ':i. \V::3 l l l f 'i |;:3:3 t it::'.'; :3:; :!filll&33iij m. a* - - * - -^' i : 3,-4 :; ; ,, .A r _ . -4 f ;- /v - r - - k '-- i--T-:j 1. 1 O ...... 1--- f I'''"'' y__'3651_ 366 __ 367 . 368 - _368_.. 370 371 372 Dau 413.00 "1 Os' 4`j .... ' 373: ` 7- 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 3.0e-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 Page 1 Set Rdbk 14.0 14.0 1.0 -2 10 2 14.0 14.0 2.0 700 8 9 11 -695 Rdbk 84.9 682.4 0023 p . 28 In order to verify mass resolution, a calibration check is performed on the mass spectrometer using a Nal/Rb/Cs tuning solution. The tuning solution is infused onto th mass spec using an infusion pump set to a flow rate o f 10 (iL/min. An MS scan from 80 to 1380 amu is performed on both M SI and MS2. The calibration! is considered acceptable if the following 11 peaks are found within 0.2 amu o f their known masses on both MSI and MS2: 84.9, 132.9, 172.8, 322.7, 472.6, 622.5, 772.4, 922.3, 1072.2, 1222.1 and 1372.0. If any o f the masses are outside the 0.2 amu, then the instrument w ill be recalibrated and another calibration check performed. The printouts from the calibration check can be found on the following 2 pages. 0024 J ^ 3 03055f8 Research Drive ^ m s tSataite College, PA 16801, USA VT: 800.281.3219 F: 814.272.1019 exygen.com p. 29 0025 p. 30 0026 p . 31 Exygen Study No.: Set No: Extraction Date: Analyzed on: L6767 111805A 11/18/05 11/18/05 Initial Calibration Curve The first curve of the data set is used to determine performance. A linear regression (with no weighting) is performed using the first eight standards of the analytical run. The coefficient o f determination (R Square) must be 0.985 or greater. If the set fails to meet this requirement, the run must be rejected and the samples reanalyzed. Exygen ID X C 110705-1 X C 110705-2 XC 110705-3 X C 1 10705-4 XC 110705-5 XC 110705-6 XC 110705-7 XC 110705-8 S ta n d a rd C o n cen tratio n (ng/L) 5 10 25 50 100 250 500 1000 SUMMARY OUTPUT Peak Area 494 826 2065 3584 7752 16331 35308 69493 Coefficient of Determination: 0.999502113 Regression Statistics Multiple R 0.999751025 R Square 0.999502113 Adjusted R Square 0.999419132 Standard Error 584.264172 Observations 8 ANOVA Regression Residual Total ______ L_ i 6 7 SS MS 4111709682 4111709682 2048187.736 341364.6227 4113757870 F 12044.92032 3.85766E-11 Intercept X Variable 1 Coefficients 167.9081974 69.33491465 tStat 257.1792017 0.652884045 0.631756937 109.7493523 P-value 0.538027981 3.85766E-11 Lower 95% -461.3870993 67.78905998 Upper 95% 797.2034941 70.88076932 -461.3870993 67.78905998 797.2034941 70.88076932 0027 p. 32 LOD and LOQ Determination Exygen Study No.: Set No: Extraction Date: Analyzed on: L6767 111805A 11/18/05 11/18/05 The height o f the first 5 ng/L standard of the analytical run is measured in centimeters and recorded. The height of the noise in a one minute range before the PFOA retention time in the reagent control is measured in centimeters and recorded. The noise height is then divided by the standard height. The result is converted to to ng/L by multiplying by the concentration of the standard measured (5 ng/L). The LOD is calculated by taking 3 times the signal to noise ratio in ng/L . The LOQ is calculated by taking 5 times the LOD. Concentration Height Exygen ID____________ (ng/L)_______ (cm) X C110705-1 5 15.1 Reagent Control ____________ 0____________ 4,5 I Signal to Noise Ratio = [height of the noise in the reagent control (cm) / height of the 5 ng/L standard(cm)] x 5 ng/mL Signal to Noise Ratio (ng/L) = LOD = LOQ = 1.490 4.47 22.4 ng/L ng/L ng/L I 0028A 002SC Quantify Calibration Report S t u d y N o . : L 6 7 6 7 , S e t N o . :1118 0 5 A , Ext.Date:ll/18/05, Analyst:K.Risha Page 1 Exygen Research, 3058 Research Drive, State College, PA 16801 0029 Quantify Sample Report Study No.:L6767, Set No .:111805A, E x t . D a t e :1 1 / 1 8 / 0 5 , Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: Printed: P : \ D a t a \ L C M S M S 7 \ M a s s l y n x \ 0 08 Mon Nov 21 06:36:20 2005 P:\Data\LCMSMS7\Masslynx\008 W e d Dec 01 06:25:13 2004 Mon Nov 21 06:44:55 2005 APFO.PRO\SampleDB\111805A APFO.PRO\MethDB\112204 PFOA Initials _ Date__ Run# A Name: 111805A-1001 Text: 1 : PFOA Page 1 Exygen Research, 3058 Research Drive, State College, PA 16801 0030 Quantify Sample Report S t u d y N o . : L 6 7 6 7 , Set N o . : 1 1 1 8 0 5A, Ext.Date:11/18/05, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P : \ D a t a \ L C M S M S 7 \ M a s s l y n x \ 0 0 8 A P F O .P R O \ S a m p l e D B \ 1 1 1 8 0 5 A Mon Nov 21 06:36:20 2005 P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\112204 PFOA Wed Dec 01 06:25:13 2004 Printed: Mon Nov 21 06:44:55 2005 Name: 111805A-1002 Text: 1: P F O A Page 2 Exygen Research, 3058 Research Drive, State College, PA 16801 0031 Quantify Sample Report S t u d y N o .: L67 6 7 , S e t N o . : 1 1 1 8 0 5 A , Ext.Date :11/18/05, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P : \ D a t a \ L C M S M S 7 \ M a s s l y n x \ 0 0 8 A P P O .P R O \ S a m p l e D B \ 1 1 1 8 0 5 A Mon Nov 21 06:36:20 2005 P:\Data\LCMSMS7\Masslynx\008 APPO.PRO\MethDB\112204 PFOA Wed Dec 01 06:25:13 2004 Printed: Mon Nov 21 06:44:55 2005 Name: 111805A-1003 Text: 1: P F O A Page 3 Exygen Research, 3058 Research Drive, State College, PA 16801 0032 Quantify Sample Report Study No.:L6767, Set N o .:111805A, Ext.Date:ll/18/05, AnalystsK.Risha Sample Lists P : \ D a t a \ L C M S M S 7 \ M a s s l y n x \ 0 0 8 A P F O .P R O \ S a m p l e D B \ 1 1 1 8 0 5 A Last modified: Mon Nov 21 06:36:20 2005 Method: ^ P: \ D a t a \ L C M S M S 7 \ M a s s l y n x \ 0 0 8 A P F O . P R O \ M e t h D B \112204 PFOA Last modified: W e d Dec 01 06:25:13 2004 Job Code: Printed: Mon Nov 21 06:44:55 2005 Name: 111805A-1004 Text: 1 : PFOA Page 4 Exygen Research, 3058 Research Drive, State College, PA 16801 p. 40 Quantify Sample Report Study No.:L6767, Set N o .;111805A, Ext.Date:ll/18/05, Analyst:K.Risha Sample Lists P : \ D a t a \ L C M S M S 7 \ M a s s l y n x \ 0 0 8 A P F O .P R O \ S a m p l e D B \ 1 1 1 8 0 5 A Last modified: M o n Nov 21 06:36:20 2005 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\112204 PFOA Last modified: W e d Dec 01 06:25:13 2004 Job Code: Printed: M on Nov 21 06:44:55 2005 Name: 111805A-1005 Text: 1 : PFOA Page 5 Exygen Research, 3058 Research Drive, State College, PA 16801 0034 p. 41 Quantify Sample Report S t u d y N o . : L 6 7 6 7 , S e t N o . :1 1 1 8 0 5 A , E x t . D a t e :11/18/05, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111805A Last modified: Mon Nov 21 06:36:20 2005 Method: P : \ D a t a \ L C M S M S 7 \ M a s s l y n x \ 0 0 8 A P F O .P R O \ M e t h D B \ 1 1 2 2 0 4 P F O A L a s t modified: Wed Dec 01 06:25:13 2004 Job Code: Printed: Mon Nov 21 06:44:55 2005 Name: 111805A-1006 Text: 1: P F O A Page 6 Exygen Research, 3058 Research Drive, State College, PA 16801 0035 p. 42 Quantify Sample Report S t u d y N o .:L 6 7 67, Set N o . : 1 1 1 8 0 5 A , E x t . D a t e :1 1 / 1 8 / 0 5 , Analyst:K.Risha Sample List: P : \ D a t a \ L C M S M S 7 \ M a s s l y n x \ 0 0 8 A P F O .P R O \ S a m p l e D B \ 1 1 1 8 0 5 A Last modified: M o n Nov 21 06:36:20 2005 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\112204 PFOA Last modified: W e d Dec 01 06:25:13 2004 Job Code: Printed: M o n N ov 21 06:44:55 2005 Name: 111805A-1007 Text: 1: P F O A XC110705-6, 250 ng/L standard 111805A-1007 Sm (Mn, 2x2) 100- %- 5.34 16331"! 18-NOV-2005 15:14:08 LC/MS/MS #7 MRM of 1 Channel ES413 >369 2.48e5 Area O1 11111111'1111 11 11'' M ' 11i' | 1i 1| 11i i | 111....................... * i " ` i ' i 1177"i " 11i 1111i Time 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 0036 p. 43 Quantify Sample Report Study No.:L6767, Set No.:111805A, Ext.Date:ll/18/05, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P :\Data\LCMSMS7\Masslynx\008 Mon Nov 21 06:36:20 2005 P:\Data\LCMSMS7\Masslynx\008 W e d Dec 01 06:25:13 2004 A P P O .P R O \ S a m p l e D B \ 111805A APFO.PRO\MethDB\112204 PFOA P r iQ t ed: Mon Nov 21 06:44:55 2005 Page 8 Name: 111805A-1008 Text: 1 : PFOA XC110705-7, 500 ng/L standard 111805A-1008 Sm (Mn, 2x2) 100- %: 5.34 18-NOV-2005 15:30:56 LC/MS/MS #7 MRM of 1 Channel ES413 >369 5.30e5 Area <y 1.00 2.00 3.00 n "T I I I I I I IT 11 11 1 1' ^ 1"r '1111 1 1111 1 1111 111 1 1111 Tim e 4.00 5.00 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 0037 p. 44 Quantify Sample Report S t u d y No.:L6767, Set No .:111805A, E x t . D a t e :1 1 / 1 8 / 0 5 , A n a l y s t s K . R i s h a Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS7\Masslynx\008 Mon Nov 21 06:36:20 2005 P:\Data\LCMSMS7\Masslynx\008 W e d Dec 01 06:25:13 2004 APFO.PRO\SampleDB\111805A APFO.PRO\MethDB\112204 PFOA Printed: Mon Nov 21 06:44:55 2005 Page 9 Name: 111805A-1009 Text : 1 : PFOA XC 110705-8,1000 ng/L standard 111805A-1009 Sm (Mn, 2x2) 100- %- 5.33 694931 18-NOV-2005 15:47:40 LC/MS/MS #7 MRM of 1 Channel ES413 >369 1.06e6 Area nu- ........................................................ I I I I 1I I , I * " '"i " " 1 " " 1 " 111 1" 1 1ime 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 0038 Quantify Sample Report Study No.:L6767, Set No.:111805A, Ext.Date:ll/18/05, Analyst:K.Risha Sample Lists P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111805A Last modified: Mon Nov 21 06:36:20 2005 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\112204 PFOA Last modified: Wed Dec 01 06:25:13 2004 Job Code: Printed: Mon Nov 21 06:44:55 2005 Name: 111805A-1010 Text: 1 : PFOA Page 10 Exygen Research, 3058 Research Drive, State College, PA 16801 0039 p. 46 Quantify Sample Report Study No.:L6767, Set N o .:111805A, Ext.Date:11/18/05, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111805A Last modified: Mon Nov 21 06:36:20 2005 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\112204 PFOA Last modified: W e d Dec 01 06:25:13 2004 Job Code: Printed: M o n Nov 21 06:44:55 2005 Name: 111805A-1011 Text: 1: P F O A Exygen Research, 3058 Research Drive, State College, PA 16801 0040 p. 47 Quantify Sample Report Study No.:L6767, Set N o .:111805A, E x t . D a t e :11/18/05, Analyst:K.Risha Sample List: Last modified: Method: ^ Last modified: Job Code: P:\Data\LCMSMS7\Masslynx\008 Mon Nov 21 06:36:20 2005 P:\Data\LCMSMS7\Masslynx\008 W e d Dec 01 06:25:13 2004 A P F O .P R O \ S a m p l e D B \ 1 1 1 8 0 5 A APFO.PRO\MethDB\112204 PFOA Printed: Mon Nov 21 06:44:55 2005 Name: 111805A-1012 Text: 1: P F O A P a g e 12 Exygen Research, 3058 Research Drive, State College, PA 16801 0041 p. 48 Quantify Sample Report S t u d y N o . : L 6 7 6 7 , S e t N o . :1 1 1 8 0 5 A , E x t .D a t e :1 1 / 1 8 / 0 5 , A n a l y s t s . R i s h a Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111805A Last modified: Mon Nov 21 06:36:20 2005 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\112204 PFOA Last modified: Wed Dec 01 06:25:13 2004 Job Code: Printed: Mon Nov 21 06:44:55 2005 Name: 111805A-1013 Text: 1: P F O A Exygen Research, 3058 Research Drive, State College, PA 16801 0042 p. 49 Quantify Sample Report Study No.:L6767, Set N o .:111805A, Ext.Date:ll/18/05, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111805A Last modified: Mon Nov 21 06:36:20 2005 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\112204 PFOA Last modified: Wed Dec 01 06:25:13 2004 Job Code: Printed: Mon Nov 21 06:44:55 2005 Name: 111805A-1014 Text: 1 : PFOA Exygen Research, 3058 Research Drive, State College, PA 16801 0043 p. 50 Quantify Sample Report Study No.:L6767, Set N o .:111805A, E x t .D a t e : 1 1 / 1 8 / 0 5 , A n a l y s t :K .R i s h a Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS7\Masslynx\008 M o n Nov 21 06:36:20 2005 P:\Data\LCMSMS7\Masslynx\008 W e d Dec 01 06:25:13 2004 APFO.PRO\SampleDB\111805A APFO.PRO\MethDB\112204 PFOA Printed: Mon Nov 21 06:44:55 2005 P a g e 15 Name: 111805A-1015 Text: 1 : PFOA Reagent Spk B, 500 ng/L 111805A-1015 Sm (Mn, 2x2) 100i %- 5.35 39560 18-NOV-2005 17:27:36 LC/MS/MS #7 MRM of 1 Channel ES413 >369 5.62e5 Area 1.00 2.00 3.00 4.00 5.00 6.00 7.00 T-H Tim e 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 0044 p. 51 Quantify Sample Report S t u d y N o . : L 6 7 67, Set No.:111805A, Ext.Date:11/18/05 , Analyst:K.Risha Sample List: P : \ D a t a \ L C M S M S 7 \ M a s s l y n x \ 0 0 8 A P F O .P R O \ S a m p l e D B \ 1 1 1 8 0 5 A Last modified: Mon Nov 21 06:36:20 2005 Method: P : \ D a t a \ L C M S M S 7 \ M a s s l y n x \ 0 0 8 A P F O .P R O \ M e t h D B \ 1 1 2 2 0 4 PFO. Last modified: W ed Dec 01 06:25:13 2004 Job Code: Printed: Mon Nov 21 06:44:55 2005 P a g e 16 Name: 111805A-1016 Text: 1 : PFOA L6767-1 Spk C, 5000 ng/L, DF=10 111805A-1016 Sm (Mn, 2x2) 100n %- 0 T - n --r j 1.00 2.00 5.36 41817 18-NOV-2005 17:44:19 LC/MS/MS #7 MRM of 1 Channel ES413 >369 6.28e5 Area 1111I 111J I 1I 111'1I 1111'1~1nI Tim e 6.00 7.00 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 0045 Quantify Sample Report Study No.:L6767, Set No.:111805A, Ext.Date:11/18/05, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111805A Last modified: Mon Nov 21 06:36:20 2005 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\112204 PFOA Last modified: W e d Dec 01 06:25:13 2004 Job Code: Printed: Mon Nov 21 06:44:55 2005 Name: 111805A-1017 Text: 1 : PFOA P a g e 17 Exygen Research, 3058 Research Drive, State College, PA 16801 0046 Quantify Sample Report Study No.:L6767, Set N o .:111805A, Ext.Date:ll/18/05, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111805A Last modified: Mon N ov 21 06:36:20 2005 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\112204 PFOA Last modified: W e d Dec 01 06:25:13 2004 Job Code: Printed: Mon Nov 21 06:44:55 2005 Name: 111805A-1018 Text: 1 : PFOA Page 18 Exygen Research, 3058 Research Drive, State College, PA 16801 0047 Quantify Sample Report S t u d y N o . : L 6 7 6 7 , S e t N o . :1 1 1 8 0 5 A , E x t .D a t e :11/18/05, A n a l y s t : K . R i s h a Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111805A Last modified: Mon Nov 21 06:36:20 2005 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\112204 PFOA Last modified: Wed Dec 01 06:25:13 2004 Job Code: Printed: Mon Nov 21 06:44:55 2005 Name: 111805A-1019 Text: 1: P F O A Page 19 Exygen Research, 3058 Research Drive, State College, PA 16801 0048 Quantify Sample Report S t u d y N o . : L 6 7 6 7 , S e t N o . :1118 0 5 A , E x t . D a t e : l l / 1 8 / 0 5 , A n a l y s t : K . R i s h a Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111805A Last modified: Mon Nov 21 06:36:20 2005 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\112204 PFOA Last modified: Wed Dec 01 06:25:13 2004 Job Code: Printed: Mon Nov 21 06:44:55 2005 Name: 111805A-1020 Text : 1 : PFOA Page 20 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report S t u d y N o . : L 6 7 6 7 , S e t N o .:1 1 1 8 0 5 A , E x t .D a t e : 1 1 / 1 8 / 0 5, A n a l y s t : K . R i s h a Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111805A Last modified: Mon Nov 21 06:36:20 2005 Method: P : \ D a t a \ L C M S M S 7 \ M a s s l y n x \ 0 0 8 A P F O .P R O \ M e t h D B \ 1 1 2 2 0 4 P F O A Last modified: Wed Dec 01 06:25:13 2004 Job Code: Printed: Mon Nov 21 06:44:55 2005 Name: 111805A-1021 Text: 1 : PFOA Page 21 Exygen Research, 3058 Research Drive, State College, PA 16801 0050 Quantify Sample Report S t u d y N o . : L 6 7 6 7 , S e t N o . :1 1 1 8 0 5 A , E x t . D a t e :11/18/05, A n a l y s t : K . R i s h a Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111805A Last modified: Mon Nov 21 06:36:20 2005 Method: P : \ D a t a \ L C M S M S 7 \ M a s s l y n x \ 0 0 8 A P F O .P R O \ M e t h D B \ 1 1 2 2 0 4 P F O A Last modified: Wed Dec 01 06:25:13 2004 Job Code: Printed: Mon Nov 21 06:44:55 2005 Name: 111805A-1022 Text: 1 : PFOA Page 22 Exygen Research, 3058 Research Drive, State College, PA 16801 0051 p. 58 Quantify Sample Report Study No.:L6767, Set N o .:111805A, E x t .D a t e : 1 1 / 1 8 / 0 5 , Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111805A Last modified: Mon Nov 21 06:36:20 2005 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\112204 PFOA Last modified: W ed Dec 01 06:25:13 2004 Job Code: Printed: Mon Nov 21 06:44:55 2005 Name: 111805A-1023 Text: 1 : PFOA P a g e 23 Exygen Research, 3058 Research Drive, State College, PA 16801 0052 Quantify Sample Report Study No.:L6767, Set N o .:111805A, Ext.Date:11/18/05, Analyst:K.Risha Sample List: Last modified: Method: Last modified: Job Code: P:\Data\LCMSMS7\Masslynx\008 Mon Nov 21 06:36:20 2005 P:\Data\LCMSMS7\Masslynx\008 Wed Dec 01 06:25:13 2004 APFO.PRO\SampleDB\111805A APFO.PRO\MethDB\112204 PFOA Printed: Mon Nov 21 06:44:55 2005 - Name: 111805A-1024 Text: 1 : PFOA Page 24 Exygen Research, 3058 Research Drive, State College, PA 16801 0053 p. 60 Quantify Sample Report S t u d y N o . : L 6 7 6 7 , S e t N o . :1 1 1 8 0 5 A , Ext.Date:ll/18/05, Analyst:K.Risha Sample List: P : \ D a t a \ L C M S M S 7 \ M a s s l y n x \ 0 0 8 A P F O .P R O \ S a m p l e D B \ 1 1 1 8 0 5 A Last modified: Mon Nov 21 06:36:20 2005 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\112204 PFOA Last modified: Wed Dec 01 06:25:13 2004 Job Code: Printed: Mon N o v 21 06:44:55 2005 Name: 111805A-1025 Text: 1: P F O A Page 25 Exygen Research, 3058 Research Drive, State College, PA 16801 0054 Quantify Sample Report S t u d y N o . : L 6 7 6 7 , S e t N o . :1 1 1 8 0 5 A , E x t .D a t e : 1 1 / 1 8 / 0 5 , A n a l y s t : K . R i s h a Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111805A Last modified: Mon Nov 21 06:36:20 2005 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\112204 PFOA Last modified: W e d Dec 01 06:25:13 2004 Job Code: Printed: Mon Nov 21 06:44:55 2005 Name: 111805A-1026 Text: 1 : PFOA Page 26 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report S t u d y N o . : L 6 7 6 7 , S e t N o . : 1 1 1 8 0 5 A , E x t .D a t e :11/18/05, A n a l y s t : K . R i s h a Sample List: P : \ D a t a \ L C M S M S 7 \ M a s s l y n x \ 0 0 8 A P F O .P R O \ S a m p l e D B \ 1 1 1 8 0 5 A Last modified: Mon Nov 21 06:36:20 2005 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\112204 PFOA Last modified: Wed Dec 01 06:25:13 2004 Job Code: Printed: Mon Nov 21 06:44:55 2005 Name: 111805A-1027 Text: 1 : PFOA Page 27 Exygen Research, 3058 Research Drive, State College, PA 16801 0056 Quantify Sample Report Study N o .:L6767, Set No.:111805A, Ext.Date:11/18/05, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111805A Last modified: Mon Nov 21 06:36:20 2005 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\112204 PFOA Last modified: W e d Dec 01 06:25:13 2004 Job Code: Printed: Mon Nov 21 06:44:55 2005 Name: 111805A-1028 Text: 1: P F O A Page 28 Exygen Research, 3058 Research Drive, State College, PA 16801 Quantify Sample Report Study No.:L6767, Set N o .:111805A, E x t . D a t e :11/18/05, Analyst:K.Risha Sample List: P :\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111805A Last modified: Mon Nov 21 06:36:20 2005 Method: P : \ D a t a \ L C M S M S 7 \ M a s s l y n x \ 0 0 8 A P F O .P R O \ M e t h D B \ 1 1 2 2 0 4 P F O A Last modified: W e d Dec 01 06:25:13 2004 Job Code: Printed: Mon Nov 21 06:44:55 2005 Name: 111805A-1029 Text: 1: P F O A Page 29 Exygen Research, 3058 Research Drive, State College, PA 16801 p. 65 Quantify Sample Report S t u d y N o . : L 6 7 6 7 , S e t N o . :1 1 1 8 0 5 A , Ext.Date:ll/18/05, Analyst:K.Risha Sample List: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\SampleDB\111805A Last modified: Mon Nov 21 06:36:20 2005 Method: P:\Data\LCMSMS7\Masslynx\008 APFO.PRO\MethDB\112204 PFOA Last modified: Wed Dec 01 06:25:13 2004 Job Code: Printed: Mon Nov 21 06:44:55 2005 Page 30 Name: 111805A-1030 Text: 1: P F O A XC110705-8,1000 ng/L standard 111805A-1030 Sm (Mn, 2x2) 100-1 % 5.35 72903 18-NOV-2005 21:38:22 LC/MS/MS #7 MRM of 1 Channel ES413 > 369 1.07e6 Area 1.00 2.00 3.00 4.00 5.00 6.00 7.00 Time 8.00 Exygen Research, 3058 Research Drive, State College, PA 16801 p. 66 Precise Research. Proven Results. p . 67 The following pages are exact copies o f information for the standards used in this study. Pentadecafluorooctanoic acid (Inventory #: SP3800), obtained from Aldrich (lot # 2 3 1 16HB) was used to make a stock solution (ID # S061605-1), which in turn, was used to make intermediate solutions (ID#'s F091305-1, F091305-2, F091305-3, F091305-4 and F 091305-5). Thse intermediate solutions are used to prepare extracted calibration standards, laboratory control samples, and matrix spike samples. Pentadecafluorooctanoic acid (Inventory #: SP5444), obtained from Oakwood Products Inc., Fluorochem U SA (lot # 203) was used to make a stock solution (ID # S040505-1), which in turn, was used to make intermediate solutions (ID#'s F091305-6 and F 091305-7). These intermedite solutions are used to prepare the check standard, which is designed as an independent source verification o f the calibration standards. The information on the following pages provides the exact sources, lot numbers, shipping information, expiration dates and storage conditions o f the neat standards. A lso included are the preparation o f stock standard and fortification solution forms. These pages show the exact details o f the preparation o f each o f the stock and fortification solutions, as well as their expiration dates and storage conditions. 0060 exygen.com RESEARCH 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 SP0003800 > 3845 Description: Pentadecafluorooctanoic acid Type: Routine Sponsor Contact: Matrix: Solids (Gravimetric) Catalog#: 171468 Lot#: 23116HB CAS #: 335-67-1 Solvent: NONE Removed: False Condition Reev'd: Room Temperature Condition Stored: Room Temperature Current Location: B1-105 Vendor: SIGMA-ALDRICH, INC. Company Name: Contact: Phone #: Notes:. Addition 5 t" * Component Withdrawal \jj s - il i C;j r - 00 iv. .l.-j m *i r: r * o C'~ o V,) & TJ K - O,,n 0.10242 0.10242 0.010244 0.010242 0.01047 0.10242 0.10242 6/21/2005 Standard Primary.rpt Units 9 Notes: 9 Notes: g Notes: 9 Notes: 9 Notes: P760 9 Notes: 9 Notes: 9 Notes: P760 S ta n d a rd s - P rim a ry ___________________________________________________________ Date Received: Expires: Special: Flammable: Health: Reactive: Gross: Gross Units: Net Balance: Net Units: 12/08/2003 12/8/2005 12:00:00AM No significant hazard Non-combustible (will not burn) Slightly toxic No significant hazard 43.03219 9 4.24186 g A liauot - SP0003800 ComDonent Puroose INITIAL Balance 14 ANALYSIS Balance 14 ANALYSIS Balance 32 ANALYSIS Balance 32 ANALYSIS Balance 17 ANALYSIS Balance 17 ANALYSIS Balance 17 ANALYSIS ComDuter BALANCE5 BALANCE5 BALANCE7 BALANCE7 BALANCE8 BALANCE8 BALANCE8 Report Version: Jun 10 2005 10:28AM Page 1 of 2 Created On 12/8/2003 12:56:03PM 12/8/2003 1:53:57PM 3/2/2004 11:45:51AM 6/1/2004 10:32:52AM 11/17/2004 11:28:49AM 11/22/2004 11:15:04AM 12/20/2004 8:17:11AM 1/19/2005 11:44:19AM Instance: Created Bv Risha, Karen Ristia, Karen Sheehan, Amy Decker, Emily Sheehan, Amy Decker, Emily Sheehan, Amy Sheehan, Amy R0173419 p. 68 |j i d U U o u u lJ > vu40 Description: Pentadecafluorooctanoic acid Type: Routine Sponsor Contact: Matrix: Catalog #: Lot#: CAS#: Solvent: Removed: Solids (Gravimetric) 171468 23116HB 335-67-1 NONE False Condition Reev'd: Room Temperature Condition Stored: Room Temperature Current Location: B1-105 Vendor: SIGMA-ALDRICH, INC. Company Name: Contact: Phone #: Notes: Date Received: Expires: Special: Flammable: . Health: Reactive: Gross: Gross Units: Net Balance: Net Units: 12/08/2003 12/8/2005 12:00:00AM No significant hazard Non-combustible (will not burn) Slightly toxic No significant hazard 43.03219 9 4.24186 9 Addition O O cn> O Component Purity Withdrawal 0.01024 0.10242 0.10242 0.10242 Aliquot - SP0Q0380Q, cont'd Units Component Purpose Computer 9 Balance 14 PREPARE Notes: g Balance 17 OTHER BALANCE8 Notes: Prepare stock for P760 g Balance 17 ANALYSIS BALANCE8 Notes: Fiuorochemicals g Balance 17 ANALYSIS BALANCE8 Notes: Stocks for fiuorochemicals. Characterization - SP0003800 Date Characterized 12/08/2003 Date Expires 12/08/2005 Characterized Bv Sigma-Aldrich Created On 2/22/2005 9:06:53AM 5/17/2005 10:55:17AM 6/16/2005 8:18:43AM 6/20/2005 3:09:46PM Created Bv Risha, Karen Created Bv Connolly, Paul Edwards, Chrissy Sheehan, Amy Kravets, Brittany p. 69 6/21/2005 Standard Primary.rpt Report Version: Jun 10 2005 10:28AM Page 2 of 2 Instance: R0173419 IH I1III1111 BHla S IG M A -A L D R fC H ... Allentown Distribution Center ' Aldrich Chemical Conpany Inc* 950 AMBASSADOR DRIVE . Allentown PA 13104 l m SHIP TO; EXYEO RESEARCH KAREN . 3Q43 RESEARCH DR STATE C0LLE5E PA 16301 --J -.it: - The SIGMA-ALDB1CH Family # SIG M A Biochemical and Reagent forLife Science Research Fluka SpecialtyChemical and Analytical Reagents forResearch Q ALDRICH- Organic and Inorganics for Chemical Synthesis LaboraCoryChemicals and Reagents for Research and Analysis SUPELCO Chromatography Products forAnalysis and Purification ALL SALES ARE EXPRESSLY LIMITED TO AND CONDITIONED UPON THE TERMS AND CONDITIONS APPEARING ON THE FRONT AND BACK OF THIS FORM. SIGMA-ALDFUCH BRANO PRODUCTS ARE SOLD THROUGH SIGMA-ALDRICH, INC. . I _! 0063 S H i P P E D F R O r i ' A LL e n t o w n Customer Service B0O-325-310 - SIGMA-ALDRICH T e c h n i c a l Service- - _ EXVGEN RESEARCH li KAREN -3T0A4AO3 RESEARCH DR STATE COLLEGE PA 14801 AIRBORNE GROUND . SP30O O 5$ g THIS PACKAGE CONFORPIS TO 49 CFR 1 7 3 .4 wmmm pu?5NW FROM A6A6L19LLD50ER0-N3ITC9AOH1MW-B9CNA1HS,0SE7APMDAIOCRA1L8D1RCBOS TO: - -- -- - ^ 5^ . 7 EXYGEK RESEARCH KAREN 3848 RESEARCH DR REF# S8T1A49T3E88C6O2LLEGE PA ORICIN * ABE c 46275417462 ADDITIONAL INFORMATION 46275417462 81493886 4B3IKR18 Trick 1:46275417462 Document 4614939682 PH O N E: 3 1 4 -7 7 1 -5 7 6 5 4031KR10 J/ k. W EIG H T(LB S) 003 P IK E S ' ZIPCODE 16801 12/05/2003 GGGGGGGGGGGGGGGGGGG SERVICE DELIVERY DAY SPECIAL HANDLING SERVICES Q46275417462 A IR B O R N E EXPRESS 2 .5 8 LBS 1 OF 1 n *3.5.91 CU9S 91/82 5P3&CO S IG M A -A L O R IC H CertficateoiAnalysis Product Name Product Number CAS Number Molecular Formula Molecular Weight TEST APPEARANCE INFRARED SPECTRUM TITRATION GAS LIQUID CHROMATOGRAPHY TITRATION QUALITY CONTROL ACCEPTANCE DATE Pentadecafluorooctanoic acid 17,146-8 335-67-1 C8HF152 414.1 SPECIFICATION WHITE TO OFF-WHITE POWDER CONFORMS TO STRUCTURE AND STANDARD AS ILLUSTRATED ON PAGE 507B OF EDITION I, VOLUME 1 OF THE ALDRICH LIBRARY OF FT-IR SPECTRA'. 95.5% - 104.5% (WITH NAOH) 95.5% (MINIMUM) 2% H 20 (MAXIMUM) LOT 23116HB RESULTS WHITE CRYSTALLINE POWDER CONFORMS TO STRUCTURE AND STANDARD 101.1% (WITH NAOH) 97.7% 0.06% H 20 (WITH 'KARL FISCHER' REAGENT) JUNE, 2003 Ronnie J Martin, Supervisor Quality Control 0065 uM6 RCH 3058 Research Drive State College, PA 16801 p. 73 SP 3000 Phone: 814-272-1039 Fax: 814-231-1580 Protocol No.: _____________ _ Exygen Study No: ___________ STUDY TELEPHONE/COMMUNICATIONS-LOG Page t o f / Person: Ken Company: Aldrich Originator Date: Time: Exygen___ x Sponsor ____ 12/08/03 1022 Notes: I called Aldrich tech service at 1-800-231-8327 to ask the shelf life o f the PFOA standard 1 received today. Ken, an Aldrich rep in technical service, told me that the shelf life is 2 years from the date o f receipt stored at room temperature._____________________ 0066 August 7, 2001/1 3058 Research Drive S tate College, PA 16801 RESEARCH Phone: 814-272-1039 Fax: 814-231-1580 PREPARATION OF STOCK STANDARD SOLUTION 'Project'" ' : Exygen Study / Project Number >Customer Project Number NJK Primary Standard Compound Name: ftivk^ertiiluoronr+orioic. A c id tV fo (\) Purity: ' . . . ' ,:v H : : '' Exygen Inventory ID: . SP0003200 Primary Standard Expiration Date: . % l7l0%}0S Stock Solution Preparation ^ v " Net W t of Compound: Net W t Adjusted for Purity: 0, l024Zg OADbOO g Final Volume: Stock Solution Concentration: I OD mL l DQO pg/rnL Solvent Exygen Inventory ID: Solvent Name: V fn n iQ ll 3 ______________ ___________________________________ Stock Solution ID: Stock Solution Expiration Date: (S M M D D Y Y -1,2,3, etc.) O to l\o OS ' \ IZ ID A S Storage Condition and Edcatlorfc w ; Freezer ID: Refrigerator ID: 3 3 Room Temperature: -- Walkin Freezer ID: -- Walkin Cooler ID: - Storage Cabinet: -- (E nter the Instrum ent or R oom ID un der the appropriate condition) 'Remarks . ' '-UP'V' ; . ' Slanature: ( J)7T M LIBRARY ID: V0000986-5 --' 0067 Date: f ) b ilb l S ~ LABORATORY FORM RESEARCH 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 \':~ ::\-r-r.- 'V`L"i-' Y-'r'V/J \,,`.T',V r S ta n d a rc isi^ P rr^ I3P0005444 > 5480 Description: Pentadecafluorooctanoic acid Type: Routine Sponsor Contact: Matrix: Solids (Gravimetric) Catalog #: 001319 Lot#: 203 CAS #: 335-67-1 Solvent: NONE Removed: False Condition Reev'd: Room Temperature Condition Stored: Refrigerated Expires: Special: Flammable: Health: Reactive: Gross: Gross Units: Net Balance: Net Units: Current Location: B1-105 / IN0000678 - Walkin Cooler 9 / D0002222 - Walkin Cooler 9 Vendor: OAKWOOD PRODUCTS, INC. Company Name: Contact: Phone #: Notes: The standard was stored in Refrigerator 33 until the Certificate of Analysis was received. Y.,V'> 3/31/2007 12:00:00AM Unknown Unknown Unknown Unknown 66.10590 9 4.98989 9 Addition 5 Component Balance 14 Withdrawal 0.01011 Units 9 Notes: 9 Notes: Aliquot - SP0005444 Component Purpose INITIAL Balance 14 PREPARE Computer BALANCE5 Characterization - SP0005444 Created On 3/18/2005 7:06:35AM 4/5/2005 1:50:15PM Purity 99% Date Characterized 03/31/2005 Date Expires 03/31/2007 Characterized Bv NA Created Bv Sheehan. Amy 00 yr-` Created Bv Sheehan, Amy Edwards, Chrissy p. 75 --- IT CD 4/8/2005 Standard Primarv.rDt Report Version: Feb 14 2005 4:43PM Page 1 of 1 Instance: R0158155 IIIIIIIVIIIIIIINIIIIIII1I1IIIIIII p. 76 Oakwood Products, Inc 741 Old Dunbar Road WestdOlumbia, SC 29172 Phone{803)739-8800 Fax(B03)739-6957 CERTIFICATE OF ANALYSIS Date: Material: Cat, No.: Cai No.: Lot No.: Assay: 3-31-05 PeBtadecafluorooctaaok acid 1319 [33S-<57-l1 263 99+% by NaQH Titration Appearance: Colorless, low-melting solid VVu kave Dot preformed a standardized stakiUty test on this componnd. We have stored this compound at room tempera cure in a tightly scaled container for many y ean and not noticed any ill effects. as. Ytunei Yang QC Manager ID'd IT:,- I g ;a c l j? ,( 0069 ww-- w G A K W O O D PRODUCTS, INC. FLUOROCHEM USA 1741 OLD DUNBAR ROAD WEST COLUM BIA. SC 2 9 1 7 2 Phone: 803-7 3 9 -8 5 0 0 FAX: 803-7 3 9 -6 9 5 7 BILL Exygen Research TO: i3 53 Research Drive State Co__egG, PA 16301 (314) 231-6032 . Page 1 p. 77 S p s -y y if 4915S O R D E -R SHIP TO: Bxygen Research AT T N : AKY 3117 Research Drive Stare College, PA 16301 !S 14) 231-3032 0070 b p S W S1- riotre OAKWQOD PP.GD5 J. S a im le 17*11 OLD D'JIIBAR RO WEST CDL.Ur.WIA, SC 29172 UNITED STATES To: Esyger R e s e a t AMT 3117 R=sar^h D-ree State CQlecje. PA 16801 UNITED STATES 'JlUClM: CAE Serwft-T t t r S9S7AS1I POSTS SEE'] 16801 Tel. ^14-331-90132 j Description: DO IM EXCEPTFD OUANTUES . Day 17TH Vigi-- 1 fos far 1 sea Dale; 2QUS-CI3-15 DHL sandsnitenrcf and eafdltla>is appb; 2LUS16801 W CEA 3Q ABH B25412924655 WAYBILL: 25412024655 (Nay Hagai able) 0071 II 3058 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 PREPARATION OF STOCK STANDARD SOLUTION Project ' -V :. Exygen Study / Project Number Nk Customer Project Number Nh Primary Standard : i; : :i'u ' ... Compound Name: Exygen Inventory ID: ^txtiodtco&uoroodttno\c- Act'd (Yfbfc) Spooo5HH4 Purity: Primary Standard Expiration Date: . % 0 3 |3 l|o 1 Stock Solution Prparation ; v :r'-.y : : " Net Wt. of Compound: 0-010U Final Volume: IDO Solvent Exygen Inventory ID: ' " R E OO 1 ft 2 0 S Net WL Adjusted for Purity: q 0.0I0O I q Stock Solution Concentration: mL IDO pg/mL Solvent Name: *, , H cm onol Stock Solution ID: (S M M D D Y Y -1 ,2 ,3 , etc.) SOHO5 0 5 - | Storage Condition and Location Stock Solution Expiration Date: , :;X.V ------------P --0--H-\P~5l0I lp . . - .------ Freezer ID: -- Walkin Freezer ID: Refrigerator ID: .8 3 Room Temoerature: - Walkin Cooler ID: -- Storaqe Cabinet: (E n ter th e Instrum ent o r R oom ID un der the appropriate condition) -- -- * Remarks. ' ` ' ''.`j tV'! i Y._ ; S o u rce , o f T F o A is Oakwcod T V cd ud s. C E E onjos'jos' ^ ulaloS . Signature: Ifo j it . LIBRARY ID: V0000986-5 0072 Date: m J o s/x;. LABORATORY FORM p. 80 t I 3058 Research Drive I S tate C ollege, PA 16801 Phone:814-272-1039 Fax: 814-231 -1580 RC H ' PREPARATION OF FORTIFICATION STANDARD SOLUTIONS Project - . v ! : .v, . . txyg e n Study / Project Number P4lb Customer Project Number .Fortification Solution Preparation , - > /, , , H^2 6^nbmM&;o1iinS:am^mbirie^iM^teihmcinbind\s^k;Viriihabrar.ktV uate Prepared: . Fortification Solutions. Expiration Date: Solvent Exygen Inventory ID: . lilo e io s Solvent Name: . . ' _____ Z____________________________________ I M - l b ______________ Initiai Soin. ID Compound Description Initial Soin. Cone. (pg/mL) Initial Soin. Allquoted Volume (mL) M erH A tJoL- Final Soin. Final Soin. Volume Cone. (mL) (pg/mL) Final Soin. ID (FMMDDYY-1,2,3, etc.) ' O klbC S ' 1 P f K to o o 10 too IDO F M l 2 0 S - l F (fl I5 0 S -1 P R A IC O 10 iD O lO F (fl O S '2 . F \\lb S - 0 - P fo A pcf l i n t s - L - ifc A P f /\ io 1.0 o .| lo 10 10 1 0Q , 1 ... l . o loo .1 lo o -0\ F i i S - 3 F q i S ' Li' F(f{\Z o s - S 5 6 4 o 5 fo -| P M \b 0 1 .0 IDO 1 .0 f '< n i3 6 S - b c im -t, ---- t P ftA -- -- M> '-- -- 10 -- -- IDO 0.1 F O T i s - 7 -- -- F-- -- --F --- -- -- -- F' Storage Condition:and Location r ` ;; \ -: Freezer ID: -- Refrigerator ID: 3 3 Room Temperature: -- Walkin Freezer ID: - Walkin Cooler ID: - Storaqe Cabinet - (Enterthe Instrument or Room ID under the appropriate condition) Remarks .. . . ; ..... ^ . : (j)SDU DF R b K VS t& W x b T ^ b J c r s . t ^ ^ | l g > | c ^ Signature: LIBRARY ID: V0000987-4 OJ 0073 Date: LABORATORY FORM
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