Document gb1o9eMOkenOBG57y1No3gg6q

ATTACHMENT C jbm ittal to 0804-013 76 000175 V . VCl ."Wv KO ;* 1 I Vi. O November 11, 2003 Ms. Lynn Hall GE Plastics 2148 North 2753rdRoad Ottawa, 1L 61250 Dear Lynn, I have attached a copy o f the C8 report. Please let me know if I can provide any additional information. Regards, Tom Livesey \ / AlgoflonPTFETechnical Service 000176 Analytical Report Fluorpchemical Characterization ot Wastewater Samples , Solvay Solexis PFOA Sampling 3/03 Exygen Research Laboratory Report No. L34300 Testing Laboratory Exygen Research 3058 Research Drive State College, PA 16801 Requester Warren H. Buck, PhD. Solvay Solexis 10 Leonard Lane Thorofare, NJ 08086 PAGE10FS ,3100558 Research Drive State College, PA 16 8 01 , USA V,T: 800.281.3219 . P : 814.272.1019 exygen.com 000177 U O / V O / V O VIE.U X O . 1 V t A A ' a 0 4 4 / O ir 4 WHt 1 Introduction Results are reported for the analysis of water samples received by Centre Analytical Laboratories, Inc. (dba Exygen Research) (Exygen) from Solvay Solexis. This report presents results assigned to Exygen Research study number L34300. Specific fluorochemical characterization by liquid chromatography / tandem mass spectrometry (LC/MS/MS) was requested for all samples. A single sample was received for analysis. The samples were prepared and analyzed by LC/MS/MS for the following list of fluorochemicals: Table 1: Target Analysis Compound Name Perfluorooctanoic Acid Acronym PFOA 2 Sample Receipt The sample was submitted in a plastic container, at ambient temperature. No sample collection date was supplied. The sample was received on 3/14/03. 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 14 days of receipt. 4 Methods - Analytical and Preparatory 4.1 LC/MS/MS 4.1.1 Sample Preparation for LC/MS/MS Analysis W ater samples were initially treated with 200 uL of 250 mg/L sodium thiosulfate solution to remove residual chlorine. Solid phase extraction (SPE) was used to prepare the samples for LC/MS/MS 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. PAGE 2 OF5 000178 UO/U O/U O VHL*' i l ) i l l i l i 49 / D0 >r<x igjuuo 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 on 3/26/03 and analyzed on 3/27/03 and 3/28/03. Raw analytical data can be found In Attachment D. 5 Analysis 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 >_0.992 (r2 > 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 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. 5.3 Surrogates Surrogate spikes are not a component of the LC/MS/MS analytical method. 5.5 Duplicates The sample was analyzed in duplicate. Results are given along with the sample results In Attachment A. 5.6 Laboratory Control Samples Milliq water was spiked with PFOA at 50 and 500 n g /L with each extraction set. All laboratory control samples showed recoveries between 70 and 130%. 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 PFOA. PAGB30F5 000179 U / U / u o nui* 1 0 : i x t a a ^ i ^^h o / o o vrt lfc.1Uk'O 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: Chain of Custody 8.3 Attachment C: LC/MS/MS Raw Analytical Data 9 Signatures Other Lab Members Contributing to Data Karen Smith 000180PAGE4 OFS U O / U O / U t f ru n / I V . i l i'A A enE w g R E S E A R C H Precise Research. Proven Results. Analytical Resiilts Solvay Solexis W astewater Sampling 3/03 Solvay Solexis Sarriple Identification PFOA (ng/L) 03083 03083 (laboratory duplicate) 74000 75100 Limit of Detection (LOD) for i l e procedure is appoxim ately 10 ng/L Limit of Quantitation (LOQ) for the procedure is 50 ng/L ND - Compound not detected NQ - Compound detected at a level between the LOD and LOQ. Result is not quantifiable. ND < LOD < NQ < LOQ X .3058 Research Drive State College, PA 16801, USA V.TF: :881144.2.27321.1,1053890 000181 exygen.com y u / u o / u y y\nyj l u . u r / \ A 4 i j i i V * V. SOLVAY SOLEXiS March 13, 2003 ^ 'SVV John Flaherty Exygen Research, Inc, 3058 Research Drive State College, FA 16801 DearJohn: I have enclosed a sample of wastewater from one of our Algoflon PTFE latex customers. I have given it the code 03083, I would like to have it analyzed for perfluorooctanoic acid (PFOA), in duplicate, Based on waste water samples from PVDF lattices that I have analyzed, I would guess that the concentration might be in, the range of tens of parts per million, but I don't know specifically what the customer's process is. Please send the results to me, and bill Accounts Payable under purchase order #1230707. Please call if there arc any questions about the request Sincerely, 030^3 Warren H. Buck, Ph. D. Analytical Services Manager -S t/Z d v j / / < //!< -*' 2 JTC 10 L E O N A R D L ANE T H O R O F A R E , NJ DS0U P H O N E : 856. Z51 - J 4 45 FAX: 85 -J 8 4 - !i 167 000182 u o / u o / u o nun taa 4 1 0 4 4 0 / 0^9 vrv^ RESEARCH 3058 Research Drive State College, PA 16801 Phone: 800-281-3219 Fax: 814-272-1019 Laboratory Sample Log-in Sheet (Environmental) Complete upon sample receipt: Client and/or Protect Name Method of Delivery Walk-in Tracking #: j y / v 'a -j Pick-up UPS J f/i,}' / < / r / S t rj p-FSdEx Air Borne Other (explain) Chain of Custody Temperature Preservation Custody,Saals: GHfresent, ^Slntacl / broken (explain) absent Thermometer ID: Cooler ID: /?,*-* Cooler ID: Cooler ID: Cooler ID: J** Cooler temp: Cooler temp: Cooler temp: Cooler temo: /'V- C C "C "C Chgjo-of-Gustody Record; 'Q present absent Samples Received: on ice in ice melt with ice pack p-fiom?"' Explanation Completed by Stonatura: ---- Date (Time): l// Complete during sample log-in: LIMS Log-in # Physical Condition Samples intact? Chain of Custody Samples received agree with COC record? Analysis Request Preservation Analysis request Clear? Sample containers appropriate? Chemical preservation appropriate? Samples received within holding time? Sample volume/mass adequate? 3 ^ 3 `fJ o e tsJes Q No (explain) S J fe s No (explain) O J e s No (explain) Yes No (explain) Yes No (explain) Yes No (explain) Yes No (explain) E xplanation Completed by Sianature: *------ Date: ?/>y / J,-3 / Complete following resolution of any nonconformances: Client Contacted Yes Client: No Resolution Data (Time): Completed by Sionature: Lab Sx Log-in Sheet -Ex Date: 11-5-01/0 000183 V U / v o / v u Mi i i i / J . U . l i , r A A O `i `i 9 / J i O XV LOGIN CHAIN OF CUSTODY REPORT (lnOl) Mar 14 2003, 03:22 pm Login Number: L34300 Account: 2980 SOLVAY SOLEXIS HSJ v jl w Page 1 Signature Date 000184 UB/ U8 / U 0 VYD I t K l J RAA 4 1 J 4 4 /2 0 vre iaj v u RAW DATA REPORT Sponsor Study No: Exygcu Study No; Analyte; ISoitnes: Monitored: NA L34300 6P1F3O-A> 369 NA Limit of Quantitation: Injection Volume: Matrix: Semple Volume: Final Volume; SOng/L l5|iL Water 40.0 mL 5.0 mL Set No; Analyse Instrument Type: Extraction Date; Analyzed on: 032603B SOLVAY Karen Risha LQMS/MS Unit # 7 03/26/03 03/27-28/03 Std. Exygca XC03ID1703-0 XC031703-1 Sponsor ID a- Sample Code Run No. C CS 032603B-3001 032603)3-3002 ConC. (np/L) 0 25 XC031703-2 XC031703-3 -- CCSS 032603B-3003 032603B-3004 50 100 XC031703-d XC031703-5 XC031703-6 - -- CS 0326Q3B-3005 250 CS 032603B-3006 500 CS 032603B-3007 1000 Methanol Wash 0106020 Control 0106020 Spk A - NA NA c LCc S 032603B-3008 O32603I3-3009 032603B-3010 - 0106020 SpkB NA LCS 032603B-3011 - L34300-1 L3430Q-1 Rep XC031703-1 XXCC003311770033--32 XC031703-d XC031703-5 XC031703-6 0033008833 - S CsS CS 032603B-3012 032603B-3013 003322660033BB--33001145 - 25 50 CS 032603B-3016 100 W - CCCSSS 00O333222G66000333BBB---33300011I987 250 500 1000 PFOA Found (ng/L) = (peakMet - intercept) / slope x DF Recovery (*) = fPFQA found (ng/LyPFOA found in control (nc/L)]_____ x 100 amount PFOA added (ag/L) Dilution Factor - -- - -- 1 1 1 100 100 - - Peak Area 0 1254 2231 141779029 24453 4BG96 0 0 2670 4231609873739013109 25870737 14527 29s56 59342 Amount PFOA PFOA Foubd Added Recovery (ng/L) (og/Ll <*) -- - - - - -. - -'- --- ND 48.9 499 50 500 9B 100 74000 . 75100 - - -. - --- --- --- --- --- Smndard Curve : Linearfl/> weighted! Intercept = 50,0803 Slops = 53.5769 Coef. Of Det. = 0 98613 CS == Calibration standard SCa=SaCmopnlterol sample LF = Lab fortified sample Fir = Field fortified sample LCS = Laboratory Control Spike CK = Check Standard ND NQ = Not detected = = Not quantifiable Response between 0 and LOD = Response between LOD and LOO Spreadsheet prepared by: U u B l # s 000185 UDZU/uo nui; 0:10 jtaa 410449/ 0^0 vjtl .SOLVAY SOLEXIS March 13, 2003 UJL JEoxhyngFenbhReersreyarch, Inc. 305BResearch Drive State College, PA 16801 , DearJohn; wthaestceIowhdaeavt0eer3e0sn8acm3l.opsleIedswaforosuamlmd PplilVkeeDotFof wlhaaatstviteceewistacathenaratlfyrIozhmead,voefonarenpaolefyrzofleuudro,rAIolwogcootfuallondnogicuFeasTdsFdtBh(aPltaFttOehxeAcc),uosnintcoemdnuetprralsit.cioa1tneh.maviBegahgstievbdeenoiinnt tqthhueeesrrtaeinosugnlestsaobftootuemtnsteh,oeafrnepdqaurbtesisllpt eArcmcoilulinotns,PbauytaIbdleonu'ntdkenrowpusrcphedasfiecaolrlydewrh#a1t2th3e07c0u7st.omPeler'assperocaclelsisfist.hePrleeaasereseanndy Sincerely, AWnaarlryetnicHal.SBeurvdisc,ePshM. aDn.ager Sc *) 10 LEONARD LANE ' THOROPARE, NJ 0S08S PHONE: 54-251-3445 FAX: S56-3-i ) i 7 000186 u o / u o / u o WEdU I D . J.O f A A `U 0 4 4 0 1 D D rv t J v J.O 3058 Research Drive State College, PA 16801 Phone; 814-272-1039 Fax: 814-231-1580 SAMPLE TRANSFER SHEET Protocol Number; Exygen Sample # L34300-1 NA_________ Exygen Study Number:_______L34300 Sponsor Sample # 03083 Exygen Sample # _ Sponsor Sample # .. _ . ,,- _ -- ,, _- _ -_ __ -_ _ -, _m _ -- -- A rV ^ SYl 0 3 / Zjp j Q 3 Requested By (Printed Name/Date/Time) Samples removed from: )de* _______ Box# Samples removed from:_________________________ Box# Samples transferred to the custody of. Samples received from custodian; Samples moved to Samples removed from______ r * f - ^ _______ , Samples returned to....................psi'oqfp ty-' c&) rx a ,l}C } W fa Comments: Shelf# Shelf# Sample Custodian Initials/Date/Timc i 0 3 ll4 /o 3 123S~ Laboratory Per: nel Initials/Date/Time y > //to Sample Custodian Initials/Date/Time December 19, 2002/6 000187 UO/ u o / u o TTE-U J.0 . 1 Ht r AA < /1 1 0 4 4 0 0 ^ 9 vrv/ `l u i * i 3058 Research Drive 1R ES A RC H State College, PA 16801 Phone: 814-272-1039 Fax:814-231-1580 Internai Chain of Custody/Fortification Sheet Exygen Study Number: L34300 Matrix: Wastewater Sponsor Study/Prgtocol No: NA 32TThime sea.mpileZsylisOted below were removed from refrigeDraattoer0N*o>.j?.U>fO- 3 Initials-- A m P . CLIENT SAMPLE ID EXYGEN ID NUMBER VOLUME (mL) I FORTIFICATION (ng) na 0106020 Control 40.0 - na 0106020 Spk A 40.0 2.0 na 0106020 SpkB 40.0 20.0 03083 L34300-1 40.0 - 03083 L34300-1 Rep 40.0 - - - -- - _ -- . - -- -- . -- - -- - __ - - .. - - - . -- -- - -- - -- -; - --- 0106020 Spk A 0106020 SpkB Spiking Solution Used P010603-4 (10 nfmL) FOI0603-3 (100 ug/inU -. -. -- -- -- All samples were measured: Time / * / / O_____ Date OPilZiajci ? Volume Used for Spiking 200 uL (200 mL micropipet) 200 pL (200 pL micropipet) * - Initials A fy lfP Initial/Date ju t 2 L \ & . L? m. - After Time. measuring / VJQ samples werei DreatuternedDto3 r!eZfrrnbigeir0at3or No. 3Z Initials Amp, C o m m e n ts: 200 nL of 250 tag/mL sodium thiosulfate was added to all samples before spiking, laltisis/Date: P rfY lP i Analysis Summary: Data Set: Data Set: ~~ Data Set:_____~_______ IIInnniiitttiiiaaalllsss///DDDaaattteee:::____**_*'___//____~_. Set extraction/analysis data verified by: Date: July 26, 2001/6 000188 000189 ^ tm I i Research Drive R C H State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 SAMPLE EXTRACTION AND ANALYSIS TRACKING SHEET EXYGEN STUDY NMUAMTBREIXR:: LW3a4s3tQew0 ater ANMAELTYHTOEDS:: 0F1FMO-A008-Q46't> PROTOCOL NUMBER: NA Client ID na na na 03083 03083 - -- - Exygen ID 0106020 Control 0106020 Spk A 0106020 SpkB ST1EP ST2EP D(miluL--t/imonLs) - ST3EP D(milLu>t/imonLs) ST4--EP -- - L34300-1 L3430O-1 Rep 1r Vro Vio >r ~ - - - .. - -- - __ _ - -- - -__ - -- - - - - - -* - - - - "- - - ._ - -. - -. - -. - . RMeaatgeerinatlss/ Xfahanol C18SPE TypeIWat _ _ _ _ _ - Initials/Dale _ . Lot# Q2^5025! NA _ _ _ - A m ft^ zu h ? , - - - -- _- - - - .- - * _- - - - .- - -- . - - - -- . -- . - - - -- - -__ - - HPLC- - -. - ___ - - -- - -.- Methanol 423o22ifti - - -. .- _ - . . - AjUDOohiQiAcetate Type! water r t lNHAl h Am s- - - - *Im lia h/D at V b iV iirt Q3^Zulo3> SSSSTTTTEEEEPPPP 3421:::: FSLLPiCCnE//aMMlcvoSSol//uMMlummSSneracentlaoaenla5yanls-myiussLpis.collected in 15 mL polypropolene tubes - m il -- -- - nitiali/D ate ^Initials and date under each step indicates the personnel that performed this step. $ $Method of Analysis for the Determination of Ammonium Perfluorooctanoate (APFO) in Water COMMENTS: 37Final extracts stored in refrigerator , Initials: Date: Q ^ jZ lfj $ 3 M y 19,2001/4 070 / OfcfrCTfc VVJ TrT ! QT iTWU 0 0 / 0 0 / 0 0 c c h c 000190 3058 Research Drive R C H State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 PREPARATION OF EXTRACTED CALIBRATION STANDARDS Exygen study NO. Protocol No.: None Method No.: 01M-008-046* Exygen Study No.: NA Analytes: PFOA Matrix: Type I Waters Sample Vol: 40 mT. Sponsor Sample ID NA Exygen Sample ID 0106020 Sample Description Type I Water' Fort. Fort. Fort, Micropipet Fort. Solution Soin. Cone. Volume used Level ID /ne/mLi fuL) fuLl fppt) Final SIoDlu#t*io*n -. XC031703-0 Reagentsf Materials Methanol Lot# 42 35 St NA 0106020 Type I WaterA FOI0603-4 10 100 200 25 XC031703- C 18 SPE NA 0106020 Type I WaterA FO10603-4 10 200 200 50 XC031703-2 Type I Water NA NA 0106020 Type I Water' F0106Q3-4 10 400 200 100 XC031703-3 - - NA 0106020 Type I WaterA FQ10603-3 100 100 200 250 XC031703-4 _ NA 0106020 Type I WaterA F010603-3 100 200 200 500 XC031703-5 - NA 0106020 TypeIWatexA F010603-3 100 400 200 1000 XC031703-6 - - NA 0106020 Type I WaterA F010603-6 100 100 200 250 XC031703-7 c# , ,, - - - - - - - - - Initials/Date: Vertical arrows in a column indicate identical values. **This must be a unique number. Use this system: Extracted Calibration Soln ID If: XCMMDDYY-0,1,2,3. etc. Samples removed from refrigerator l freezer # o2- Time: 1005 Initials/Date: tEK / sjl'iJR 40 mL of each sample measured using a 50 mL graduated cylinder. After measuring, samples returned to refrigerator I freezer # , Time: 1460 Samples fortified: Initials/Date:__ tyj-- /03)ll\b2> SPEclean-up: Initials/Date: I Initials/Date: f'FR Initials/Date:f fR I Rlrijrrt I 3}n|o^ TH IS IS AN EXACT COPY OF TOEORIGINALI____ B ___ W ) f> g rf,C 3r2^]o^ Final volume adjusted to 5 mL: Extracts placed in refrigerator # o'! Initials/Date: /*H / -4)n|r.s Initials/Date; eft, / 3in jcR STANDARD EXPIRATION DATE: 3/31/03 Comments: AThis type I water has been filtered through a hypercarb filter * Method of Analysis for the Determination of Ammonium Perfluorooctanoate (APPO) in Water. July 10,2001/0 en/ftn/on t? a C7 t >> H a aIS! r MassLynx - Sample List Sample Usi: Signature: Printed: C:\MassLynx\fluorochemicats.pro\SampleDB\032603B SOLVAY.SPL By CENTRE\Karens (Karen Risha) At Thursday, March 27,2003 3:44:36 PM Reason Create Sample list Friday, March 28,2003 9:20:48 AM Kl'tVWMjg, Vial 23451697811111111111023645798 4123676659666234657123245 File Name LIMS ID 000000000000000000033333333333333333332222222222222222222666666666666666666600000000000000000003333333333333333333BBBBBBBBBBBBBBBBBBB------------------3-3333333333333333330O0000000000000000000000000011111111111423689703524598617 -- -- -- -- -- -- -- -- -- -- -- -- -- ... -- -- Client ID -- ... -- -- --. -- -- -- -- ... -- -- -- -- -- -- -- ... Sample Description Matrix XCQ31703-0,0 ng/L Standard XC031703-1, 25 ng/L Standard XC031703-2, 50 ng/L Standard XC031703-3,100 ng/L Standard -- XC031703-4, 250 ng/L Standard -- XC031703-5, 500 ng/L Standard -- XC031703-6,1000 ng/L Standard -- Methanol Wash -- 0106020 Control 0106020 Spk A, 50 ng/L 0106020 Spk B, 500 ng/L L34300-1, DF=100 L34300-1 Rep, DF=100 XC031703-1,25 ng/L Standard XC031703-2, 50 ng/L Standard XC031703-3,100 ng/L Standard -- XC031703-4, 250 ng/L Standard -- XC031703-5, 500 ng/L Standard -- XC031703-6,1000 ng/L Standard -- u o / u o / u o uniU o ; j . o r m /4 1 0 4 4 0 0 ^ 0 Exygen studyno. IJ tM Page 1 of 2 Page Position (1,1) Sample Type Cone (ng/L) Cone B Cone C Test ID DF Standard Standard Standard Standard Standard Standard Standard Blank Blank QC QC Analyte Analyte Standard Standard Standard Standard Standard Standard 0 25 50 100 250 500 1000 -- _ 50 500 -- -- 25 50 100 250 500 1000 _ . . . 0,000000 1.000000 -- . . . 0.000000 1,000000 -- -- 0.000000 1.000000 . . . -- 0.000000 1.000000 -- -- 0.000000 1.000000 -- --- - 0.000000 1.000000 -- -- 0.000000 1.000000 -- -- 0.000000 1.000000 -- . . . 0.000000 1.000000 -- -- 0.000000 1,000000 -- . . . 0.000000 1.000000 -- -- 0.000000 100.000OOO ... -- 0.000000 100.000000 -- ---- 0.000000 1.000000 ... -- 0.000000 1.000000 -- -- 0.000000 1.000000 ------ -- 0.000000 1.000000 -- -- 0.000000 1.000000 -- --- 0.000000 1.000000 vr^ i^ u k 000191 Mass Lynx - Sample List Sample List: Signature: Printed: C:\MassLynx\fIuorochemicals.pro\SampleDB\032603B SOLVAY.SPL By CENTRE\Karens (Karen Risha) At Thursday, March 27,2003 3:44:36 PM Reason Create Sample list . Friday, March 23,2003 9:20:48 AM W jdnaLi, MS Method HPLC Method MS Tuna File Inj Volume PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA PFOA Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water Water PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOA Tune PFOATune PFOATune PFOATune PFOATune PFOATune PFOATune 15,000000 15,000000 15.000000 15.000000 15.000000 15.000000 15,000000 15.000000 15.000000 15.000000 15,000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 15.000000 0 7 0 / O frTrfT* V V J Q T ' QT rT3 U 0 0 / 0 0 / On Exygen study N@. Page 2 of 2 Page Position (2,1) 'IJA CTnrSl 0 0 1 9 2 UQ/ UO/ UO unx/ l . i u rA A 4 X 0 4 4 0 / o ^ o vrt IfcfJ VXiT LC/MS/MS SYSTEM AND OPERATING CONDITIONS Sponsor Protocol No: NA Exygen Study No: L3430Q Instrument: Micromass Quattro Ultima (LC/MS/MS Unit #7) Computer. IBM IntelliStation M Pro Software: Windows XP Professional: Version 5.1: Service Pack 1 Micromass Limited: MassLynx 4.0 HPLC Equipment: Hewlett Packard (HP) Series 1100 HP Quat Pump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column: Genesis C -8,5 cm x 2.1 mm i-d. x 4 p (Exygen ID: 72A) (JONESCHROMATOGRAPHY: Part No. FK5962E) Mobile Phase (A) : 2 mM Ammonium Acetate in Type I Water Mobile Phase (B) : Methanol Analyst: PEK30hxa5oyr8negneeR:nRe(Rs8ise1eha4sare)cah2r7cD2hr-1iv0e3,9StFatAeXC:o(l8le1g4e), 2P3A1-115688001 NOTE: Titnhhseetrmnueamxssteln3ytnpsxaegsttoeisfntgwasraeurcseoepdmrfopogurrtaethrmeg.aenTneahrleyasptieasdgoepfsrtichnoitsnodtuaatistnaftrshoeemt. All Handwritten Peak ID's by: 000193 U O / U O / U TT1/ X U . i . U f M rrv Experiment Report File: c:\massiynx\fluorochemicals.pro\acqudb\pfoa.exp Signature: At By Reason Thursday, March 27,2003 14:13:39 CENTREVKarens (Karen Risha) update solvent delay Printed: Thursday, March 27, 2003 14:50:03 itywtu Page 1 Name Creation Time Instalment Identifier Version Number Duration (min) Calibration Filename Solvent Delay Start 2 Solvent Delay End 2 Solvent Delay Temperature 2 Solvent Delay Divert Valve Enabled Number Of Functions Default Experiment Thu 27 Mar 2003 14:13:39 1.0 8.0 C:\MassLynx\calibration.pro\ACQUDB\NalRbCs032603.cal 8.0 1105.0.0 1 Function 1 : MRM of 413.00->369.00, Time 0.00 to 8.00, ES- Type MRM Ion Mode ES- Parameter File c:\masslynx\default.pro\acqudb\default.ipr Inter Channel Delay (sec) Span (Da) Start Time (min) 000...100 End Time (min) 8.0 Ch Prnt(Da) Dau(Da) Dwell(s) Cone(V) Coll(eV) Delay(s) 1 413.0 369.00 0.20 10.00 10.00 0.03 000194 VO/UO/VU WEJL/ 1Q.1Z r/lA /0,60 vrv^ Method Report Method File; Last Modified; gnature; Printed; C :\MassLynx\008-apfo.pro\ACQUDB\Water Thursday, March 27, 2003 14:09:50 At Wednesday, March 26, 2003 13:07:14 By CENTRE\karans (Karen Risha) Reason create HPLC method Thursday, March 27, 2003 14:50:56 i^/j i | HP1100 LC Pungp Initial Conditions Solvents A% B% C% Dfc 60.0 40-0 0.0 0.0 Plow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature LeCt(C) Oven Temperature Right<C) 0.300 1S.0 0 400 35.0 35.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 10 entries which are ; Time A% 0.00 0.40 1.00 7-00 7 .SO 9.00 9.50 13.50 14.00 15.00 B% 60.0 60.0 10.0 10-0 0-0 0.0 60.0 60.0 60.0 60.0 C% 40.0 40.0 90.0 90.0 100.0 100.0 40.0 40.0 40.0 40-0 D% Plow (ml/min) Pressure 0.0 0.0 0.300 0.0 0.0 0.300 0.0 0.0 0-300 0.0 0.0 0.300 0.0 0.0 0.300 0.0 0.0 0.400 0.0 0.0 0.400 0.0 0.0 0.400 0.0 0.0 0.300 0.0 0.0 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 Contaetl Off Off Off Off 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 ( p l / m i n ) Draw Position (mm) Stop Time (mine) Injection Volume (/il) Vial Number Thermostat On Thermostat Temperature(C) 200.0 200 0.10 15.00 15.0 1 12.0 1JV61 Page 1 400 400 400 400 400 400 400 400 400 400 000195 u o / u o / u o a u -LO ILt f A A 4 X 0 4 4 9 / 0 ^ 0 vr^ Tune Parameters File: C:\MassLynx\fluorochemicals.PRO\ACQUDB\PFOA Tune.lPR Signature: At By Reason Thursday, March 27, 2003 14:01:08 CENTRBKarens (Karen Risha) new tune file Printed: Thursday, March 27,200 3 14:51:17 H*J Page 1 Type Daughter Scan Source (ES-) Capillary (kV) Cone (V) Hex 1 (V) Aperture (V) Hex 2 (V) Source Tem perature (C) Desolvation Temperature (C) Cone Gas Flow (L/Hr) Desolvation Gas Flow (L/Hr) A n a ly s e r LM 1 Resolution HM 1 Resolution Ion Energy 1 Entrance Collision Exit LM 2 Resolution HM 2 Resolution Ion Energy 2 Multiplier (V) Pressure Gauges Pirani Pressure(mbar) Penning Pressure(mbar) MUX C onfiguration Probe Start Mass 367 S e ttin g s 3.00 10 0.0 0.0 0.0 100 300 131 669 S e ttin g s 15.0 15.0 1.0 -2 10 2 15.0 15.0 2.2 700 1.146-3 OFF Standard End Mass 372 Readbacks -2.94 -11 Set Mass 413 100 300 Readbacks 8 9 11 -696 000196 r>" u e / u a / u o vjj rAA 4 1 0 4 4 0 /0 ^ 0 vrv^ Quantify Calibration Report Study No.;L34300, Data Set;032603B SOLVAY, Ext.Date:03/26/03, Analyst;K.Risha i Dataset: S^nature: printed: C:\MassLynx\fIuorochemicals.pro\032603B SOLVAY.qld At Friday, March 28.2003 9:07:08 AM By CENTRE\Karens (Karen Risha) Reason Processing Friday, March 28, 2003 9:07:19 AM |i Method: C:\MassLynx\fluorochemicals.PRO\MethDB\PFOA 032603.mdb 28 Mar 2003 08:18:18 tijf Calibration: 28 Mar 2003 08:49:19 I Compound name: PFOA ' Correlation coefficient: r - 0.993045, rA2 0.986138 Calibration curve: 53.5769 * x + 50.0803 L Response type: External Std, Area [; Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None IV-1 u Page 1 of 1 000197 U D / U O / U O n vrr x o . x o t a a n o ' i ' i o i u i i j t1V t Quantify Sample Report Study No.:L34300, Data Set:032603B SOLVAY, ExtDate: 03/26/03, Analyst:K.Risha If Dataset: ` .^nature: C:\MassLynx\fluorochemicals.proVQ326Q3B SOLVAY.qld At Friday, March 28, 2003 9:07:08 AM By CENTRE\Karens (Karen Risha) Initials Date Method: C:\MasRseLaysnoxntfluPororocecshseinmgicals.PRO\MethDB\PFOA 032603.mdb 28 Mar 2003 08:18:18 :!; CPrainlitberda:tion: 28 FMriadray2,0M03ar0c8h:4293:,129003 9:07:19 AM : Name: 032603B-3001 Date: 27-Mar-2003 " Time: 21:23:58 Description: XC031703-0,0 ng/L Standard Page 1 of 19 Exygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 000198 ..Piuiw ''U,J,,i [' IM .U f,,l.*U P !^>U! 'n19M9> u o / u o / y o W EU J . . 1 ) r A A `i i y - H O i V A O Ti v_- Quantify Sample Report Study No.:L34300, Data Set:032603B SOLVAY, Ext.Date:03/26/03, Analyst:K.Risha Dataset: 'nature; Printed: C:\MassLynx\fluorochemicals.pro\032603B SOLVAY.qld At Friday, March 28, 2003 9:07:08 AM By CENTRE\Karens (Karen Risha) Reason Processing Friday, March 28, 2003 9:07:19 AM Name: 032S03B-3002 Date: 27-Mar-2003 Time: 21:40:40 Description: XC031703-1, 25 ng/L Standard PFOA Page 2 of 19 Exygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 000199 Quantify Sample Report Study No.;L34300, Data Set:032603B SOLVAY, Ext.Date:03/26/03, Analyst:K,Risha Dataset: Signature: Printed: C:\MassLynx\fluorochemicals.pro\032603B SOLVAY.qld At Friday, March 28, 2003 9:07:08 AM By CENTRE\Karens (Karen Risha) Reason Processing Friday, March 28, 2003 9:07:19 AM Name: 032603B-3003 Date: 27-Mar~2003 Time: 21:57:17 Description: XC031703-2, 50 ng/L Standard PFOA D32603B-3003 $mooth(Mn,2x3) XC031703-2,50 ng/L Standard PFOA 5.15 Page 3 of 19 MRM of 1 channel,ES413 >369 <ygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 000200 U O / U O / U rrjDt/ r / i A 4 1 0 1 *1 ^ 1 0 ^ 0 uv ja n tify Sample Report Udy No.:L34300, Data Set;032603B SOLVAY, Ext.Date:03/26/Q3`, Analyst:K.Risha jtaset; gn?` : inted: C:\MassLynx\fluorochernicals.pro\032603B SOLVAY.qld At Friday, March 28,2003 9:07:08 AM By CENTRE\Karens (Karen Risha) Reason Processing Friday, March 28, 2003 9:07:19 AM ame: 032603B-3004 ate: 27-Mar-2003 me: 22:13:54 escription: XC031703-3,100 ng/L Standard "OA I2603B-3004 5mooth(Mn,2x3) 1031703-3,100 ng/L Standard PFOA S.1S Page 4 of 19 MRM of 1 channel,ES413 >369 :ygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 000201 U 0 / U 3 / U 0 T i t t U i O : ^ U JTAA 4 1 0 4 4 0 I U ^ 0 uvy ; Q uantlf/ Sample Report ,Study No.:L34300, Data Set:032603B SOLVAY. Ext.Date:03/26/03, AnalystK.Risha Dataset: S' ''tlire: ? printed: C:\MassLynx\fluorochemicals.pro\Q32603B SOLVAY.qld At Friday, March 28, 2003 9:07:08 AM By CENTRE\Karens (Karen Risha) Reason Processing Friday, March 28,2003 9:07:19 AM Name: 032603B-3005 Date: 27-Mar.2003 Time: 22:30:43 Description: XC031703-4,250 ng/L Standard PFOA 032603B-30Q5 Smooth(Mn,2x3) XC031703-4,2S0 ng/L Standard PFOA S.1S Page 5 of 19 MRM of 1 channel,ES413 >369 Exygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 000202 Quantify Sample Report Study No.;L34300, Data Set;032603B SOLVAY, Ext.Date:03/26/03, Analyst.'K.Risha Dataset: Si' *ure: Printed: C:\MassLynx\fluorochemicals.pro\032603B SOLVAY.qld At Friday, March 28, 2003 9:07:08 AM By CENTRBKarens (Karen Risha) Reason Processing Friday, March 28,2003 9:07:19 AM Name: 32603B-3006 Date: 27-Mar*2003 Time: 22:47:27 Description: XC031703-5, 500 ng/L Standard PFOA 032603B-3006 Smooth(Mn,2x3) XCQ31703-5, 500 ng/L Standard PFOA 5.15 Page 6 of 19 MRMof1channel.ES413 >369 Exygen Research. 3058 Research Drive, State College, PA 16801 Data acquired on LCMSMS#7 000203 vv / UO/ \JO TTEtU l U . i i l r A A V tmU rx v Quantify Sample Report Study No.:L34300, Data Set:032603B SOLVAY, Ext.Date;03/26/03, AnalystK.Risha Dataset; Si ure: Printed: C:\MassLynx\fluorochemicals.pro\032603B SOLVAY.qld At Friday, March 28,2003 9:07:08 AM By CENTRBKarens (Karen Risha) Reason Processing Friday, March 28,2003 9.07:19 AM Name: 032603B-3007 Date: 27-Mar-2003 Time; 23:04:17 Description: XC031703-6,1000 ng/L Standard PFOA 032603B-30O7 Smooth(Mn,2x3) XC031703-B, 1000 ng/L Standard PFOA 5.15 Page 7 of 19 MRM of 1 channel,ES413 > 369 Exygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 000204 V O / O O / O it njQj\j i u . i i' a a I K lantify Sample Report idy No.:L34300, Data Set:032603B SOLVAY, Ext.Date:03/26/03, Analyst:K.Risha taset; jnature: nted: C:\MassLynx\fIuorochemicals.pro\032603B SOLVAY.qld At Friday, March 28, 2003 9:07:08 AM By CNTRE\Karens (Karen Risha) Reason Processing Friday, March 28, 2003 9:07:19 AM me: 032603B-3008 te: 27-Mar-2Q03 ne: 23:20:57 scription: Methanol Wash OA 603B-300B Smooth(Mn.2x3) Page 8 of 19 MRM of 1 channel,ES- jen Research, 3058 Research Drive, State College, PA 16801 Data acquired on LCMSMS#7 000205 luantify Sample Report ;tudy No.34300, Data Set;032603B SOLVAY, Ext.Date:03/26/03, AnalysfcK.Risha Jataset: iigr 'e; rinted: C:\MassLynx\fluorochemicals.pro\032603B SOLVAY.qld At Friday, March 28, 2003 9:07:08 AM By CENTRE\Karens (Karen Risha) Reason Processing Friday, March 28, 2003 9:07:19 AM lame: 032603B-3009 late: 27-Mar-2003 Ime: 23:37:41 Ascription: 0100020 Control *FOA 32603B-3009 Smooth(Mn,2x3) Page 9 of 19 MRM of 1 channel.ES- ixygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 000206 y u / u y / v u M l j J > X U tm hi i. X W X tV I V teV Quantify Sample Report Study No.34300, Data Set;032603B SOLVAY, Ext.Date:03/26/03, Analyst:K.Risha Dataset: Signature; Printed: C:\MassLynx\fluorochemicals.pro\032603B SOLVAY.qld At Friday, March 28, 2003 9:07:08 AM By CENTRE\Karens (Karen Risha) Reason Processing Friday, March 28, 2003 9:07:19 AM Name: 032603B-3010 Date: 27-Mar-2003 Firne: 23:54:25 Description: 0106020 Spk A, 50 ng/L PFOA 032603B-3010 Smooth{Mn,2x3) 0106020 Spk A, 50 ng/L PFOA 5.1S Page 10 of 19 MRN/I of 1 channel,ES413 > 369 <ygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 000207 U /U O /U J T XXJ X \ i . U im t \ J X I \J U V Q uantify Sample Report Study No.:L34300, Data Set:032603B SOLVAY, Ext.Date:03/26/03, Analyst: K.Risha Dataset; Signature: Printed: C:\MassLynx\fluorochemicals.proV032603B SOLVAY.qld At Friday, March 28, 2003 9:07:08 AM By CENTREtKarens (Karen Risha) Reason Processing Friday, March 28,2003 9:07:19 AM Name: 032603S-3011 Date: 28-Mar-2003 Time: 00:11:12 Description: 0106020 Spk B, 500 ng/L PFOA 032603B-3011 Smooth(Mn,2x3) 0106020 Spk B, 500 ng/L PFOA 5.15 Page 11 of 19 MRM of 1 channel,ES413 >369 Exygen Research, 3058 Research Drive, State College, PA 16801 Data acquired on LCMSMS#7 000208 Quantify Sample Report Study No.;L34300, Data Set:032603B SOLVAY, Ext.Date:03/26/03, Analysts,Risha Dataset: Signature: Printed: C:\MassLynx\fluorochemicals.pro\032603B SOLVAY.qld At Friday, March 28, 2003 9:07:08 AM By CENTRE\Karens (Karen Risha) Reason Processing Friday, March 28, 2003 9:07:19 AM Name: 032603B-3012 Date: 28-Mar~2003 Time: 00:27:58 Description: L34300-1, DF=100 PFOA 032603B-3012 Smooth(Mn,2x3) L343O0-1, DF100 PFOA 5.14 Page 12 of 19 MRM of 1 channel,ES413 >369 Exygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 000209 Quantify Sample Report Study No.34300, Data Set:032603B SOLVAY, Ext.Date:03/26/03, Analyst:K.Risha Dataset: Sianature: Printed: C:\Massl_ynx\fluorocfiemicals.pro\032603B SOLVAY.qld At Friday, March 28, 2003 9:07:08 AM By CENTRE\Karens (Karen Risha) Reason Processing Friday, March 28, 2003 9:07:19 AM Name: 032603B-3013 Date: 28-Mar-2003 Time: 00:44:47 Description: L34300-1 Rep, DF=100 PFOA 032603B-3013 Smooth(Mn.2x3) L.34300-1 Rep, DF100 PFOA 5.U Page 13 of 19 MRM ot1 channel,ES413 > 369 Exygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 000210 y u / w v? / m m Tf liJW X W . .W l ' / X O . * * X W * - * W I V f c M Quantify Sample Report study No.:L34300, Data Sel:032603B SOLVAY, Ext.Date:03/26/03, AnalysttK.Risha Dataset: Slanature: Printed: C:\MassLynx\fluorachemicals.pro\0326Q3B SOLVAY.qld At Friday, March 28,2003 9:07:08 AM By CENTRE\Karens (Karen Risha) Reason Processing Friday, March 28, 2003 9:07:19 AM Name: 032603B-3014 Date: 28-Mar-2003 Time: 01:01:30 Description: XC031703-1, 25 ng/L Standard PFOA D32603B-S014 Smooth(Mn,2x3) XC031703-1,25 ng/L Standard 100- Page 14 of 19 MRM of 1 channel,ES413 >369 1,4B8e+004 0.95 S \. 4 ^T 0.50 1.00 1.79 2.20 I ii r rp -m -p- 1.50 2.00 2.50 2,09 4.17 4.48^72 I . ! I 11 i i , I>M | rvrrp, 3.00 3.50 4,00 4.50 5.00 6-31 6.44 5-'61 7.20 7,50 ...A.W W 7.94 a 1" 11" 5.50 6.00 6.50 ' " I n ' ' r-i-n mm 7.00 7,50 a.Do Exygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 000211 \j *j / \j \? / v u rrjuis v - /luck ** x I Quantify Sample Report Study No.;L34300, Data Set;032603B SOLVAY, Ext.Date:03/26/03, Analyst.K-Risha Dataset: Signature: Printed: C:\MassLynx\fluorochemicals.pro\032603B SOLVAY.qld At Friday, March 28, 2003 9:07:08 AM By CENTRBKarens (Karen Risha) Reason Processing Friday, March 28, 2003 9:07:19 AM Name: 032603B-301S Date: 28-Mar-2003 Time: 01:18:11 Description: XC031703-2, SO ng/L Standard PFOA 032603B-3015 SmoottitMn,2x3) XCD31703-2,50 ng/L Standard PFOA 5.15 Rage 15 of 1q MRM of 1 channel,ES413 >369 xygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 000212 uu/ uvj/ y; .fa** * * X V * `* ' J r I V A . V Quantify Sample Report Study No.:L34300, Data Set:032603B SOLVAY, Ext.Date:03/26/03, Analyst:K.Risha Dataset Sinnature: Printed: C:\MassLynx\fluorochemicals.pro\032603B SOLVAY.qld At Friday, March 28,2003 9:07:08 AM By CENTRE\Karens (Karen Risha) Reason Processing Friday, March 28, 2003 9:07:19 AM Name: 032603B-3016 Date: 28-Mar-2Q03 Time: 01:34:58 Description: XC031703-3,100 ng/L Standard PFOA 032603B-3016 Smooth(Mn,2x3) XC031703-3,100 ngfl. Standard PFOA 5.14 xa v v page 16 of 19 MRM of 1 channel,ES413 > 369 /gen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 000213 y u / V O / U J VlU XU - i** x a a * * x w/ -* *U * w * w Quantify Sample Report I Study No,.134300, Data Set:032603B SOLVAY, Ext.Date;03/2S/03, Analyst:K.Risha Dataset: r Signature: C:\MassLynx\fluorochemicais.pro\032603B SOLVAY.qld At Friday, March 28, 2003 9:07:08 AM By CENTRE\Karens (Karen Risha) Reason Processing I Printed; Friday, March 28, 2003 9:07:19 AM Name; 032603 B-3017 Date: 28-Mar-2003 Time: 01:51:45 I Description: XC031703-4,250 ng/L Standard I PFOA 032S03B-3017 Smooth(Mn,2x3) XC031703-4, 250 ng/L Standard 100-1 I I %- I I ' 0.50 `' ' V.00 1" 1.50 rq ' 2.00 I Page 17 o f 19 MRM of 1 channel, ES413 > 369 1.057e+O05 H1"'7.00 J " 7.50 " ' ' '8.0o',n Exygen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 000214 u u/ v ^ / v / 1Ul/ AW <* an-iA -1 S S I V J v Quantify Sample Report Study No.:L34300, Data Set:032603B SOLVAV, Ext.Date:03/26/03, Analyst;K.Risha Dataset: pi-nature: Printed: C:\MassLynx\fluorochemicals.pro\032603B SOLVAY.qld At Friday, March 28, 2003 9:07:08 AM By CENTRE\Karens {Karen Risha) Reason Processing Friday, March 28,2003 9:07:19 AM Name: 032603B-3018 Date: 28-Mar-2003 Time: 02:08:26 Description: XC031703-5,500 ng/L Standard PFOA 0326038-3018 Smooth(Mn,2x3) XC031703-5,500 ng/L Standard PFOA 5.15 page 1a of 19 MRM of 1 channel.ES413 >309 gen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 000215 UO/ UOi us rrr.v Jlu .O T A A '* > u i -' Quantity Sample Report Study No.:L34300, Data Set:032603B SOLVAY, ExtDate;03/26/03, Analysts,Risha Dataset: Signature: Printed: C:\Masstynx\fiuorocheiriicals.pro\0326Q3B SOLVAY.qld At Friday, March 28, 2003 9:07:08 AM By CENTRRKarens (Karen RIsha) Reason Processing Friday, March 28, 2003 9:07:19 AM Name: 032603B-3019 Date: 28-Mar-2003 Time: 02:25:15 Description: XC031703-6,1000 ngfL Standard PFOA 032603B-3019 Smooth(Mn,2x3) XC031703-6, 1000 ng/L Standard PFOA 5,15 Page 19 of 19 MRM of 1 channel,ES413 > 369 gen Research, 3058 Research Drive, State College, PA 16801, Data acquired on LCMSMS#7 000Z16