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Laboratory Report Analytical Report of Data for PFOSA Pharmacokinetic Study in Rats (Sera and Liver) Laboratory Report No. FACT-TOX-145 (W2814) Requester Project No. T-7132.2 Testing Laboratory 3M Environmental Technology & Safety Services 3M Environmental Laboratory Fluorine Analytical Chemistry Team (FACT) 2-3E-09 935 Bush Avenue, St. Paul, MN 55106 Laboratory Contact Kris Hansen, Ph.D. Bldg. 2-3E-09 P.O. Box 3331 St. Paul, MN 55133-3331 Phone: (651)778-6018 FAX: (651)778-6176 Requester Andrew Seacat and Deanna Luebker 3M Company Toxicology Services 220-2E-02 St. Paul, MN 1 OF6 1 Introduction T his study was designed to prelim inarily assess the adsorption and m etabolism by the Sprague D aw ley rat o f ? p S u o ^ m e S f o n y l L i d e (PFOSA, Q F n S O .N H ^ C A S # 31506-32-8). T estram os w ere d d b y oral p v a g e with 5 mg/kg o f PFO SA suspended in 2% TW EEN 80; control aran^swere given U T T O N 80 w ith no PFOSA. Subsets o f the dosed group and the control group were sacrificai on day 1, d ^ .a n d dav 29 post-dose. Sera and liver collected from the sacrificed anim als were sent to the Envuonmenral Lab and analyzed quantitatively for perfluorooctane sulfonate (PFOS, CgF^SOj', CAS # 2795-39-3), PFO SA, and perfluorooctanoate (POAA, C7F15CO2, CAS # 2991-51-7). PFOS and PFOSA were detected in the livers o f all dosed anim als. PFOS levels were highest in the day 4 group, but even liver from anim als sacrificed 29 days post dose w ere detom ined to , PFOS PFO SA levels in the livers o f the dosed anim als were highest m the group sacrificed on day 1,o n day 29, the average PFOSA level w as approxim ately 2.5 % o f the day 1 levels. PO A A was not detected above the lim it o f quantitation in the livers o f dosed anim als. A s in the liver extracts, sera extracts collected 4 days p o sp o s e evidenced the highest PFOS levels. Serum PFO SA levels decreased from day 1 to day 4 to day 29; on day 29, sera from four out o f fivearum als did not contain PFO SA above the lim it o f detection. PO A A w as detected in th e sera ofaranuds collected on day 1 and day 4. Screening studies o f the dose material suggest that a sm all amount o f POAA w as present in the PFO SA dosing solution. PFOSAB (C gFpSO ^N H , w as detected in the livers o f dosed animals. This analyte w as also present in the solution used to dose the anim als. N o investigations o f PFOSAB in the sera w ere conducted The solution used to dose the test anim als w as analyzed to confirm the theoretical dose levels. The PFO SA concentration in the TW EEN 80 solution w as determ ined to be 1330 + /- 400 pg/m L. PFOS and PO A A were also iHpntifipH in the dose solution. The concentration o f PFOS w as estim ated to be approxim ately 18.5 ug/mL- PO A A levels are approximated at 2.5 pg/m L. PFOS and POAA data were collected from a single analysis and should be considered to be o f screening quality only. A more thorough characterization o f the material used to dose the anim als w as requested by 3M T oxicology and w as conducted by Fred D eroos poor to initiation o f the study. R esults o f this more com prehensive characterization are available from the requestors. A lthough rigorous quality control measures and 3M Environmental Laboratory Standard Operating Procedures were follow ed, the acquisition o f this data w as not necessarily collected according to applicable Good Laboratory Practices. N either the dose material nor the analytical standards were given a certificate 0 analysis; dose material was characterized by NM R and LCM S and the analytical standards were characterized by N M R The data presented here is not suitable for distribution to any governm ent agency m defense o f product suitability or safety. This data is the highest quality data available at this time. 2 Sample Receipt ................... ................................. ........ On 10/6/99 10/8/99 and 11/1/99 Deanna Luebker from 3M T oxicology Services shipped rat urine, feces, liver, and sera, to the FACT group in the 3M Environmental Laboratoiy; sam ples were received frozen on dry ice and were stored at - 20 C. 3 Holding Times There is no holding tim e criteria associated w ith these sam ples for LC/ESM SM S analysis. 2 OF 6 Methods - Analytical and Preparatory A nalytical m ethods E T S -8-4.1, Extraction o f Potassium Perfluorooctanesulfonate or Other Fluorochem ical Compounds from Serum for A nalysis U sing HPLC-Electrospray/M ass Spectrometry E T S-8-6.0, Extraction o f Potassium Perfluorooctanesulfonate or Other Fluorochem ical Compounds from L iver for A nalysis U sing HPLC-Electrospray/M ass Spectrometry E T S-8-5.1, A nalysis o f Potassium Perfluorooctanesulfonate or Other Fluorochem icals in Serum Extracts U sing HPLC-Electrospray/M ass Spectrometry E T S-8-7.0, A nalysis o f Potassium Perfluorooctanesulfonate or Other Fluorochem ical on L iver Extracts U sing HPLC-Electrospray/M ass Spectrometry Sam ple preparation-H P L C /E SM SM S: ion -p airin g extraction A nalyte is extracted from sam ple matrix w ith ion pairing reagent [tetrabutyl amm onium hydrogen sulfate (TBA )] in a pH-controlled environm ent The cationic reagent selectively targets anionic fluorochem icals. O nce the anion-TB A pair is formed, the analyte is transferred into a non-polar organic solvent (m ethyl-ierfbutyl ether), dried, and reconstituted in methanol for M S analysis. H PL C /E SM SM S In HPLC, an aliquot o f extract is injected and passed through a reverse phase liquid chromatographic colum n. Based on the affinity o f the analyte for the stationary phase in the colum n relative to the liquid m obile phase, the analyte is retained for a characteristic amount o f tim e. For exam ple, in a standard solution PFOS may elute at 8.0 minutes. Retention tim es betw een a standard PFOS solution and the analyte extracted from tissue in this analysis were m atched on the HPLC system to w ithin 1%. F ollow ing HPLC separation, ESM SM S provides a rapid and accurate m eans for analyzing a w ide range o f organic com pounds, including fluorochem icals. Electrospray, an ionization technique used primarily for detection o f m olecular ions, is generally operated at relatively m ild temperatures. M olecules are ionized, and a primary ion, characteristic o f the analyte, is selected. T his ion is bombarded w ith high-energy gas; subsequent collision s create sm aller secondary ionic fragm ents unique to the primary ion, w hich are detected. For exam ple, for PFOS (Q F p S Q O analysis, ion 499 is selected as the characteristic primary ion. T his ion is fragm ented into other ions such as 80 amu (corresponding to SO3"), and 230 amu (CsFgSOj"). Each o f these secondary fragm ents is detected and can be used to differentiate PFOS from other com pounds that m ight have the same characteristic 499 amu primary ion, but different chem ical com positions and secondary ion fragmentation patterns. 4 Analysis 4.1 Calibration Quantitation o f the target analytes is based on linear regression analysis (w eighted 1/x) o f two extracted matrix curves bracketing each group o f sam ples. Quantitation o f each analyte is based in the response o f one or more specific daughter ions using the m ultiple response-m onitoring m ode o f the instrum ent A m id-level, extracted matrix calibration check standard is analyzed every 5-10 sam ples to monitor instrumental drift. Calibration check standards are com pliant if instrumental response is w ithin + /- 30% o f the expected value. 3 OF6 4.2 Blanks Two extraction blanks, utilizing water as surrogate matrix, are extracted w ith each batch o f sam ples. A dditionally, tw o sam ples o f blank matrix (both liver and sera) are extracted along w ith each batch o f sam ples and curves. Blanks are com pliant if no target analyte is detected above the lim it o f detection for a sp ecific analyte. In this study, all blanks w ere com pliant 4.3 Surrogates Tetra-hydroperfluorooctanesulfonate is used as a surrogate in this analysis. Surrogate response is m onitored to confirm gross instrumental failure, if necessary. In the non-diluted sam ples, the surrogate response w as acceptable (+/-50% ) for all analyses. 4.4 Matrix Spikes D uplicate matrix spike analyses utilizing all target analytes w ere prepared and analyzed for one control animal W ith one exception, PFOS recoveries w ere w ithin the acceptable range o f 70-130% . O ne liver matrix spike showed a 66 % recovery for PFOS. A ll PFO SA matrix spike recoveries w ere acceptable for PFOSA. A s POA A w as not a target analyte in this analysis, no matrix spikes w ere prepared A lthough the recovery ofP O A A from sera and liver has been verified for other studies, PO A A results should be considered screening quality only. One matrix spike was prepared for each o f the target analytes in the dose verification study. Spike recovery for PFO SA w as 130%, PFOS w as 115%, and PO A A w as 121%. 4.5 Laboratory Control Samples Laboratory Control Sam ples are not a com ponent o f this study. 4.6 Sample Related Comments. Other m atrices submitted w ith this study w ill be analyzed as needed upon written request from the sponsors. In the event o f further analysis, an additional report w ill be generated D ose verification w as conducted by evaluating diluted aliquots o f the dose against an unextracted standard curve. Triplicate dilutions o f the TW EEN 80 dose solution were analyzed for determ ination o f PFO SA; a single dilution w as analyzed for determ ination o f PFOS and POAA. 5 Data Summary The table o f results detailing the sera analysis is available in Attachment A. R esults o f the liver analysis are presented in Attachment B. PFOS and PFO SA were detected in the fivers o f all dosed anim als. PFOS levels w ere highest in the day 4 group, but even day 29 group anim als were determ ined to contain high levels o f PFOS. PFO SA levels in the fivers o f the dosed anim als w ere highest in the group sacrificed on day 1; on day 29, the average PFO SA level w as approxim ately 2.5 % o f the day 1 levels. PO A A w as not detected above the lim it o f quantitation in dosed anim als. A s in the liver extracts, sera extracts collected 4 days post-dose evidenced the highest PFOS levels. Serum PFO SA levels decreased from day 1 to day 4 to day 29; on day 29, sera from four out o f fiv e anim als did not contain PFO SA above the lim it o f detection. PO A A w as detected in the sera o f anim als collected on day 1 and day 4. Screening studies o f the dose material suggest that a sm all amount ofP O A A w as present in the PFO SA dosing solution. PFOSAB was detected inthe livers ofdosed animals. This analyte was also present inthe solutionusedto dose the anim als. N o investigations o f PFOSAB in the sera w ere conducted. 4 OF6 The solution used to dose the test animal: w as analyzed to confirm dose levels. The PFO SA concentration in the TW EEN 80 solution w as determined to be 1330 + /- 400 gg/m L. PFOS and PO A A w ere also identified in the dose solution. The concentration o f PFOS w as estim ated to be approxim ately 18.5 pg/m L; PO A A levels are approximated at 2.5 pg/mL. PFOS and PO A A data w ere collected from a single analysis and should be considered to be o f screening quality only. 6 Data Quality Objectives and Data Integrity N o circum stances existed during the present study that w ould have adversely affected the quality or integrity o f the data. The follow ing data quality objectives w ere follow ed during the study: Linearity - The correlation coefficient (1*2) o f the standard curve w as equal to or greater than 0.98 using 1/x w eighting Lim its o f detection (defined as 'Athe LOQ) --PFOS in sera is 4.88 ng / mL; PFOS in liver is 15.3 ng / g, PFOSA in sera is 2.47 ng / mL; PFO SA in fiver is 6 .2 ng / g Lim its o f quantitation (defined as the low est extracted standard accurate to w ithin 30% o f theoretical value) - PFOS in sera is 9.76 ng / mL; PFOS in fiver is 30.7 ng / g, PFO SA in sera is 4.93 ng / mL; PFOSA in liver is 12.4 ng / g D uplication frequency/acceptable precision - < 30% Spike frequency/acceptable recoveries - 70% to 130%; PFOS recovery w as 66 % for a single matrix spike in liver (see Section 4.4) U se o f confirmatory methods - no confirmatory m ethods were used Demonstration o f specificity - specificity w as demonstrated by chromatographic retention tim e and m ass spectral characterization o f a single product ion G iven the parameters fisted above, and assum ing spike recoveries form a suitable indication o f endogenous analyte recovery, data are quantitative to + /- 30% The validity o f this assum ption has not been verified by other techniques. 7 Attachments A ttachm ent A: T able o f results o f sera analysis A ttachm ent B : T able o f results o f liv er analysis A ttachm ent C: Sam ple receipt A ttachm ent D: Screening results o f dose verification A ttachm ent E: E xtraction and analytical data 5 OF6 8 Signatures A L isa Clem en, Advanced Chem ist -- lot* 19<? D ate & L H z -------------- ----------------------------------- Kris Hansen, Ph.D ., Principal A nalytical Investigator /-is/O b /tf* ? D ate 6 OF6 Laboratory Report Analytical Report of Data for PFOSA Pharmacokinetic Study in Rats (Sera and Liver) Laboratory Report No. FACT-TOX-145 (W2814) Requester Project No. T-7132.2 Attachment A Table of Results - Sera Analysis FACT-TOX-145 Study: Product NumbatTcst Substance): Matrix: Method'llevinoa: Analytical Equipment System Number lnaninini Software/Verxioo: Filename: R-Squared Value: Slope: Y ln texcept: Dale* of Extraction/Analyst D a ta of Analysis/Analyst: Date of Data Reduction/Analyst: TOX-145 Pharmacokinetic Study of PFOSA in Rats T-7132 2 Rat Scnuu BTS-t-4 1and ETS-l-5.1 Soup 020199, Davey 070799. Amelia 062491 Maislytu 3 3 Sec Attachments Sec Attachments Sec Attachments Sec Attachments 10/19/99, 11/03/99 SEE/MCH 10/19/99, 10/25/99, 10/27/99, 11/04/99, lt/OJ/99 MMH/IAS 10/20/99. 10/26/99. 10/21/99, ll/OS/99. 11/01/99 IAS/MMH Sim ple D ili RAT SERUM Group Dmc Somplc * PFOS Cose. ag/mL PFOS Reported ag/mL Average PFOS ug/mL Method Blk H20 BU-I0I99-M H20 Blk-10199-H 000 <LOD 000 <LOD <LOD K20 BU IIOJ9 9 H20 Blk-11039-9 000 <LOD 000 <LOD <LOD Matrix Blk RBSI0I99-Sera Blk II 000 <L0D RBSI0I99-Scra Blk-II 000 <LOD <LOD RTSI0I99-Sera Blk-ll 000 <LOD RTSI0!99-Scra Blk 12 000 <LOD <L0D RBSI 1039-Sera Blk-9 000 <LOD RBSI1039>Scra Blk-9 0.00 cLOD <LOD QC 250 ppb RTSIOI99-2SO ppb-MS-ll RTSIOI99-2SO ppb-MSD-11 231 243 93% 91% 96% RTSI1039-250 ppb-MS 9 RTSI1039-230 ppb-MSD-10 116 172 75% 69% 72% Creap 1 0 0 mg/kg 9R03230M, Dayl 9R0323IM. Dayl 9R03232M. Dayl 000 <LOD 000 <LOD 000 <LOD 9R03233M. Dayl 9R03234M. Dayl 000 <LOO 000 <LOD <LOD Group 2 0 0 mg/kg 9R032JSM. Day4 9R03236M, Day4 9R03237M, Day4 000 <LOD 000 <LOD 0 00 <LOD 9R0323IM. Day4 9R03239M. Day4 000 <LQD 000 <LOD <LOD Groop 3 0 0 IB|/1| 9R03240M. Day29 9RQ324IM, Day29 9R03242M. Day29 9R03243M, Day29 9R03244M, Day29 000 <LOD 000 <LOD 000 <LOD 000 <LOD 000 <LOD <LOD Group 4 5 0 mg/kg CroopS 50 a |/l| Groop6 5 0 mg/kg 9R03245M. Dayl 9R03246M. Dayl 9R03247M. Dayl 9R0324IM, Dayl 9R03249M, Dayl 9R032S0M. Day4 9R032SIM. Day4 9R03232M. Day4 9R032S4-IM, Day4 9R032S4-2M. Day4 9R032SSM. Day29 9R032S6M, Day29 9R032S7M. Day29 9R032SIM, Day29 9R03259M. Day29 139 694 216 101 117 935 133 665 147 7.34 122 156 771 150 74 226 113 172 161 151 7 91 162 359 359 391 3 91 404 404 413 4 13 736 736 462 Limit of QuMititmion (LOQ): PFOS 5 SS ng/mL. POAA - 49 3 ng/mL, PFOSA - 4 79 ng/mL lim it of Detection (LOD): PFOS - 1.74 af/mL. POAA - 24.7 nf/mL, PFOSA - I 51 Bg/mL D ue Eniocd'By: Date Verified/ By: 1021-99, 10/29/99, 11/05/99 LAC 11/W99GML 11/16/99 GML rsd POAA Std. Dev. MS/MSD RPD Cone ug/mL NA <LOO NA 0 00 <LOD 000 NA <LOD NA NA <LOD NA 000 <LOD 0.00 NA 5% NA NA 1% NA 000 000 000 000 <LOD 000 000 000 ooo 000 <LOD 0.00 NA NA NA <LOD NA NA 101 147 121 21 9 103 110 120 610 67.4 105 II 1 101 1.56 11 4 NA NA NA 33.4 NA 1 54 NA PFOS * PerilBorooctanenilfonatc POAA - Periluorooctaooaie PFOSA - Pcriluoropctapcsulfonamide NA - Not Applicable or Not Analyzed NS - Not Spiked POAA Reported ug/aiL NA NA <LOD <LOD NA NA NA NA <LOD <LQD NA NA NA NA <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD NA NA NA NA NA 0 101 0 147 0 121 0103 0.120 0 0610 0.0674 0 105 0 101 00114 NA NA NA NA NA Average POAA og/mL NA <LOD NA NA <LOD NA NA <LOD <LOD NA 0 121 0.014S NA RSD Std. Dev. MS/MSD RPD NA <LOD NA NA <LOD NA NA ! OD <LOD NA 146 00177 21.0 0.0177 NA PFOSA Cone. ug/mL 0450 0 320 0 450 0320 000 000 0390 0.320 000 0.00 243 264 246 24S 1 41 0 720 0330 0 340 0.300 0430 0 290 0 430 0 320 0.270 000 000 000 000 0.00 260 437 255 334 277 61 3 SI 3 753 607 39.0 0.140 1 20 1 09 1 16 501 PFOSA Rcperied ug/mL <LOD <LOD <LOD <LOD <L0D <LOD <LOD <LOD <LOD <LOD 91% 106% 99% 99% <LOD <LOD <LOO <LOD <LOD <LOD <LOD cLOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD 0 260 0.437 0.235 0334 0277 0 0613 0 0513 0.0733 0 0607 00590 <LOD <LOD <LOD <LOD 0 00501 Average PFOSA V -i<LOD <LOD LOD <LOD <LOD 102% 99% <LOD <LOD <LOD 0313 0 0629 0 00501 RSD Std- Dev. MS/MSD RPD <LOD <LOD <LOD <LOD <LOD 1% 0% <LOD <LOD <LOD 24.4 0 0761 112 0 00702 N/A ETS-l-5 I Excel Veroo 5/95 TOX-HS-tera xls / Laboratory Report Analytical Report of Data for PFOSA Pharmacokinetic Study in Rats (Sera and Liver) Laboratory Report No. FACT-TOX-145 (W2814) Requester Project No. T-7132.2 Attachment B Table of Results - Liver Analysis FACT-TOX-145 Study Product NumberfTesl Substance): Matrix: Method/Reviston: Analytical Equipment System Number Instrument Software/Versten Date o f Extraction/Analyst Date o f Analytts/Analyst Date o f Data Reduction/Analyst Sam ple Data TOX-I45 Pharmacokinetic Study ofPFO SA in Rats. T-713X2 Rat Liver ' ETS-8-6.0 and ETS-S-7.0 Soup 020199, Amelia 062498 Masslynx 3.3 ' 10/13/99, 11/04/99 SEE/RWW/SAL 10/15/99. 10/19/99 MMH, 11/05/99 IAS, 11/10/99 IAS l< y )8 /9 9 .10/2099.11/08/99,11/11/99 IAS/MMH Filename R-Squtfed Value: Slope: Y-lmeretpt See Attachments See Attachments See Attachments S ee Attachments RAT LIVER Group Dose Sample # PFOS Cale. Cone Method Blk H 20 Blk-11 0.00 000 Matrix Blk H 2 0 Blk-2 H 2 0 Blk-2 RBL10199-Uver Blk-11 0.00 0.00 0.00 0.00 RBL10199-Liver BUt-2 1.86 0.00 QC 250 ppb 9R03230M, Day 1-M S-11 9R03235M, Day4-MS-12 276 264 226 216 9R03240M, Day29-MS-l 9R03240M, Day29-MSD-2 212 191 Group 1 O.Omg/kg Group 2 O.Omg/kg 9R03230M, Davi 9R0323IM, Dayl 9R03232M, Dayl 9R03233M, Dayl 9R03234M. Dayl 9R03235M, Day4 9R03236M, Day4 9R03250M, Day4 9R03238M. Day4 9R03239M. Dav4 0.00 0.00 000 0.00 000 0.00 0.00 295 2Z0 000 Group 3 O.Omg/kg Group 4 5 .0m g/k g Group 5 5.0 mg/kg Group 6 5 .0m g/k g 9R03240M. Day29 9R03241M, Day29 9R03242M. Day29 9R03243M. Day29 9R03244M. Day29 9R03245M, Dayl 9R03246M, Dayl 9R03247M, Dayl 9R03248M. Dayl 9R03249M. Davi 9R03237M. Day4 9R03251M. Day4 9R03252M. Day4 9R03253M. Day4 9R03254M, Day4 9R03255M, Day29 9R03256M, Day29 9R03257M. Day29 9R03258M, Day29 9R03259M. Day29 0.00 000 000 0.00 000 23660 32260 36179 21200 27829 36791 32619 42606 36945 38268 20305 20638 22025 26172 29867 Limit o f Quanutauon Limit (LOQ): PFOS - 26.9 ng/g.1 Limit o f Detection (LOD): PFOS - 8.45 ng/g, PFOSA 3.50 ng/g Total Amount o f PFOS <LOD <LOD <LOD <LOD <LOD CLOD CLOD cLOD 92% 88% 75% 72% 72% 65% cLOD CLOD cLOD cLOD cLOD cLOD cLOD 0.0295 cLOQ cLOD CLOD cLOD cLOD cLOD cLOD 23.7 3X3 36.2 21.2 27.8 36.8 32.6 42.6 36.9 38.3 20.3 206 22.0 26 2 29.9 Date Entered/Analyst 1071/99. 1 0 7 2 9 9 , 11/15/99 LAC, 11/08/99 GML Date Verificd/Analyst 11/16/99 GML PFOS o t/t cLOD cLOD <LOD cLOD 90% 73% 68% cLOD cLOQ CLOD 28.2 37.4 23 8 RSD Std. Dev. MS/MSD RPD cLOD cLOD cLOD cLOD 5% 5% 10% c LOD c LOQ CLOD 21.7 6.12 956 3.58 17.3 4 12 PFOSA Calc. Cone. __________ l i __________ 0.00 0.00 0.00 0.00 0.00 0.00 0.760 0.00 313 283 229 215 352 330 0.00 0.00 0.00 000 0.00 X35 0.00 22.0 4.66 " 0.00 X57 1.72 0.724 0.162 0.00967 6021 7015 6239 6657 8811 3523 3470 3959 3454 4105 85.5 175 104 142 303 o f PFOSA ug/g CLOD cLOD cLOD cLOD cLOD cLOD cLOD 104% 94% 76% 71% 119% 112% CLOD CLOD cLOD cLOD cLOD cLOD 0.0220 cLOD cLOD cLOD cLOD cLOD cLOD cLOD 6.02 7.02 6.24 666 8 81 3.52 3.47 3.96 3.45 4.11 0.0855 0.175 0 104 0.142 0 303 RSD PFOSA Std. Dev. - _________ MS/MSD RPD cLOD 1 cLOD <LOD <LOD cLOD <LOD cLOD 99% <LOD 10*/. 74% 116% 7% 7% cLOD <LOD cLOD <LOD cLOD 695 370 0 162 <LOD 16.0 111 8.28 0.307 530 0 0859 PFOSA " Periluoroocunesulfonamide Samples numbers may have been switched 3237 should be 3250 These samples may be falsely high, due to carryover from accidentally switching 3237 and 3250 GML 11/16/99 ETS-8-7.0 Excel Vernon 5/95 TOX-145-liver.xls 11/30/99 9.33 AM Laboratory Report Analytical Report of Data for PFOSA Pharmacokinetic Study in Rats (Sera and Liver) Laboratory Report No. FACT-TOX-145 (W2814) Requester Project No. T-7132.2 Attachment C Sample Receipt A1 0 /0 6 /1 9 9 9 3M ENVIRONMENTAL LABORATORY REQUEST FOR ANALYTICAL/FIELD WORK 1 LAB REQUEST NO. W2814 REQUESTOR NAME: DEANNA LUEBKER DEPARTMENT: 0227 PROJECT NO: 0 0 1 0 5 3 5 0 0 9 DATE RECEIVED: 1 0 /0 6 /1 9 9 9 DESC: PFOSA PK STUDY IN RATS TO X-145 CONTRACT L A B (S ): EXP COMP DATE: 1 2 /3 0 /1 9 9 9 DATE COMPLETED: PROJECT LEAD: KJ HANSEN PHONE NO: 6 5 1 -7 7 8 -6 0 1 8 3M FAX NO: 6 5 1 -7 7 8 -6 1 7 6 220-2E -02.7-1374 SAMPLE DATE CODE DESCRIPTION RESULT MDL o r (95% C . I . ) 1 KJH-SPEC SPECIAL STUDY - KJH # # = UPDATED DATA I^ ^ fc5 H U K . TOX-145 SAMPLES RECEIVED d L . Barbara A. Gramenz .... 10/07/99 10:08 AM ET&SS Lab 2-3E-09 Fax: 778-6176 To: Kari J. Rambo/US-Corporate/3M/US@ 3M-Corporate Grant A. Paul/US-Corporate/3M/US@ 3M-Corporate Lisa A. Clemen/US-Corporate/3M/US@ 3M-Corporate Kris J. Hansen/US-Corporate/3M/US@3M-Corporate cc: Subject: TOX-145 SAMPLES RECEIVED On 1 0 /6 /9 9 we received 10 Liver, 10 Sera, 20 Feces and 20 Urine Samples for days 1 & 2 from 3M TOXICOLOGY. FACT-TOX-145. LAB REQUEST # W2814. PFOSAPK Study in Rats (T-7132.2). Samples received frozen on dry ice and have been stored in Freezer F-16 at 20+V10C. Barb !)/ f . f , , J ^ - / / r " C t ' f Printed 10/07/99 [3M Restricted] Page 1 PFOSA PK STUDY IN RATS TOX-145 LR# W2814 DAY 1 DATE 10/5/99 Gen. MALE POST DOSE URINE ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 FECES ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 LIVER ID# 9R03230 9R03231 9R03232 9R03233 9R03234 9R03245 9R03246 9R03247 9R03248 9R03249 SERA ID# 9R03230 9R03231 9R03232 9R03233 9R03234 9R03245 9R03246 9R03247 9R03248 9R03249 DAY 2 DATE 10/6/99 Gen.MALE POST DOSE URINE ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 FECES ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 Chain of Custody Record 3M Environmental Laboratory Form 35176 PWO 3M Facility Co^jOoroJC- ~TiC. Address XL City. Slate. Zip Code 09303 3M P ioject Title P P o S /h P/C 3M Facility Coniaci 7 LudbhLs~ 3M Telephone Number -l-fS IH 3M Rnceqquuoeasiteeir - 3M Project Lead fV vlfcM S c a c a J - 3M Project Number . T - n ^ . ^ ii/ g f t T S ~T ~7fSi7"p" O /i^if 0 7 3M Department Number 0 3 3 1 ___________ 1ab Requesl/TemplaieiJumber .............. L Z li BySam pled (Print) T y m W)^ L u c b & y ' S am oier Signature . Conlraclor Dale Number Containers of each Preservatives Item # II Sample y Description /Q /& > l Date Time Matrix 4) zCO OZzn 8 XW X0z(0 8 1 n ylft fdS o [ I n r t f , in / S a rt (JLr<rtO 2 r \ / j " 11 " it ilo Ko*1 lLr,nt> 3 D y ( FhSf Z c frrL (O K l/Orn C rrcS 4 O y O - K /' n lO lif fv s J 5 n / / PKfddiu L e fts ' /<VS L mct~ 6 ] \ f l d StrfjSL; !verzX-. (o/S c1bn\ <9 c ^ x -' 7 Total Containers of Each Item Sam ples S p lit S ee A ttachm ent Comments J_ t1 it t* a h 'r n f r ft, G SrtACfi/g rnnt^ ff _____________ ( ( Ssnylliq Pft if s1 ^ 1 5430-^3'- Cf J SrnjnUjPfi&y* 8 9 10 11 12 13 . Item # ^ ______ -- Relinquished By/Aftiliation Time >t4>/ Date ~ ' ------------------ ---------------------------------^ ------__________-- -- -- ------------------ - Shipped Via - = -------- - .........-- -- Received By/Affiliation ........................ Time .............. Date i iy- rras\nn U b k /r /^ ^ f sttU te .- X s r - Z7 O ngm al AccH'pj See Reverse Side For Instructions TOX-145 SAMPLES RECEIVED Barbara A. Gramenz 1 0 /1 1 /9 9 11:54 AM ET&SS Lab 2-3E-09 Fax: 778-6176 To: Kari J. Rambo/US-Corporate/3M/US@ 3M-Corporate Grant A. Paul/US-Corporate/3M/US@ 3M-Corporate Lisa A. Clemen/US-Corporate/3M/US@ 3M-Corporate Kris J. Hansen/US-Corporate/3M/US@ 3M-Corporate CC! Subject: TOX-145 days 3&4 SAMPLES RECEIVED On 1 0 /8 /9 9 we received 10 Liver, 10 Sera, 20 Feces and 20 Urine Samples for day 3 1 0 /7 /9 9 & day 4 1 0 /8 /9 9 from 3M TOXICOLOGY. FACT-TO X-145. LAB REQUEST # W 2814. PFOSA PK Study in Rats (T-7132.2). Samples received frozen on dry ice and have been stored in Freezer F-16 at -20+V 10C . Barb 5 r>\ j0UJ y c O ff\'c < J i u - f i - i r / j Printed 10/11/99 [3M Restricted] Page 1 PFOSA PK STUDY IN RATS TOX-145 CR# W281?^ DAY 3 DATE 10/7/99 Gen. MALE POST DOSE URINE ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 FECES ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 DAY 4 DATE 10/8/99 Gen.MALE POSTDOSE URINE ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 FECES ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 LIVER ID# SERA ID# 9R03235 9R03235 9R03236 9R03236 9R03237 9R03237 9R03238 9R03238 9R03239 9R03239 9R03250 9R03250 9R03251 ' 9R03251 9R03252 9R03252 9R03253 9R03254 g)9R03254 DN AR TUX> 5 6 S M ^ P l 5 BT TRD3<253 BUT DCaTt (jMIOMCWE. "BAe^ lo/ufc. PFOSA PK STUDY IN RATS TOX-145 LR# W2814 DAY 3 DATE 10/7/99 Gen. MALE POST DOSE URINE ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 FECES ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 DAY 4 DATE 10/8/99 Gen.MALE POST DOSE URINE ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 FECES ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 LIVER ID# SERA ID# 9R03235 9R03235 9R03236 9R03236 9R03237 9R03237 9R03238 9R03238 9R03239 9R03239 9R03250 9R03250 9R03251 9R03251 9R03252 9R03252 9R03253 9R03254 g)9R 03254 T W a r e t ic o RR33S4 5R N S M 'A p t ONG SV-U(_D B E 4\RD3 2 5 3 B u t KJOLO (jBMIOHOWE. "X ^av/i- ad.d cl -tf - 2. -V Atoe. W 4<_r* i*-- *n o-c^- "BAQ^ Chain of Custody Record 3M Environmental Laboratory Form 35176 PWO 3M Facility /c o r p m J c ^ Address ~T5s Oily. Slate. 2ip Code nQRnn 3M Project Title p fiM 3M Facility Coniaci jN T> pfr. r - 3M Telephone Number -7 /.T 7 M 3M Requester TPect-n^^ L u e b k L r- 3M Project Lead /fo itrtu J Td w z ^^f r o c c f r 3M Project Number T P n f c rJ-3. DdIpS'JJ'oH 3M Department Number yi*)! Lab Request/Tempiate Number -- - uMh I BySampled (Print) ryfxntnfjL U id h d c r ' Same 1er Signature _ 'cl1 Item # (} Sample Description Contractor Dale l lS L Date Time Matrix Number Containers of each Preservatives zco ozz a XCM NaOH Total Containers of Each Item Q S am p les S plit S ee A ttachm ent Comments 1 T \ / R f i cJ D d \ C j l l r , n C o h <7/10! U r t n O 2 ( / " >' K f r c c f r / t / 7 P p fY \ f r e e s 3 K /*1 >' " U . n n /fcft (Lnf&s 4 e 'i> f 1j - f r e e s / t / , f ^CUA i c e - 5 ' 5 r itti P o U /io S O /-V tr ' I h l f h Y tr 6 c ' " 7 " i / r A rp r 8 / jo _ /o iO _ _ZJQ _ /'O /a n i-/ > '/ ft 11 >/ 9 _ _ --------- -- ^ 10 \ Ul 11 12 13 * = = z z ------------------ Item # ! - Lp Relinquished By/Affiliation pCan/Y4 g e tta r / f r Y Time -1 ^ 5 0 Date f tfW Shipped Via Received By/Atfiliation frbad- u n r ttf' (jjr ^ /) C k n ^ ^ / l f r Time H -ocyrK Date IoI m I v Chtyirtdl Au . uii;j.j ,i> b.ui.j i. I.. ! 0 @ l a c i^ k See Reverse Side For Instructions TOX-145 day 29 SAMPLES RECEIVED Barbara A. Gramenz " 1 1 /0 2 /9 9 02:13 PM ET&SS Lab 2-3E-09 Fax: 778-6176 To: Kari J. Ram bo/US-Corporate/3M/US@ 3M-Corporate Grant A. Paul/US-Corpo/ate/3M /US@ 3M -Corporate Lisa A. Clem en/US-Corporate/3M/US@ 3M-Corporate Kris J. Hansen/US-Corporate/3M/US@ 3M-Corporate Subject: TOX-145 day 29 SAMPLES RECEIVED On 1 1 /2 /9 9 we received 10 Liver, 10 Sera Samples for day 29 from 3M TOXICOLOGY. FACT- TOX 145. LAB REQUEST # W 2814. PFOSA PK Study in Rats (T-7132.2). Samples received frozen on dry ice and have been stored in Freezer F-16 at -20+V10C . Barb yj Printed 1 1 /0 2 /9 9 [3M Restricted] Page 1 PFOSA PK STUDY IN RATS TOX-145 LR# W2814 DAY 29 DATE 11/2/99 Gen.MALE POST DOSE LIVER ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 SERA ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 Chain of Custody Record 3M Environmental Laboratory Form 35176 PWO 3 M Facility ConntsYTtJcj " 7 5 / Address 33 0 C ity, State. Zip Code 1 BySam pled (Print) D i o / 7 / l o ^ L u c io k Z jr- Sam pler Signature Item # ( / Sample Description Contractor Date U Date 1 g a d - t i\ lL T yrtn iU r AVUW 2 3 V o< L rz> ~ hl/ v l /s ( m i m i 4 / 1* 5 ---- 09305 3W Requester 3M Project Lead iu c /b ^ 3M Project Tille J_ P F o S fr PfC 3M Facility Contact in & t S L>oy-nno^ /jjc & k jL S - 3M Telephone Number -7 -/3 W toXiHb 3M Number Lab Request/Tempiate Number u u a x iH / V f 1 ________ Time Matrix Number Containers of each Preservatives Zc0 n OZX 8XCM XOZ Total Containers of Each Item S am ples S p lit See A ttachm ent Comments Oon \* 1* --< <; $ 5 6 7 8 ~ ------------- -------- 9 flTai\ i---- ------- ------- 10 11 13 .-- ------------------- -- Item # Relinquished By/Affiliation j^ J tL TXnr*A#- U cb k ^ n /T D y? Time Date Shipped Via z ceived By/Affiliation -- --------------- -- Time Date jjM ? Original At t.im pjnyiu.j Suini I. I 1 !'.I See Reverse Side For Instructions D Laboratory Report Analytical Report of Data for PFOSA Pharmacokinetic Study in Rats (Sera and Liver) Laboratory Report No. FACT-TOX-145 (W2814) Requester Project No. T-7132.2 Attachment D Screening Results of Dose Verification Kris J. Hansen 11/04/99 02:29 PM Tel: 7 7 8 -6 0 1 8 2-3E-09 y Fax: 7 7 8 -6 1 7 6 Environmental Lab To: Andrew Seacat/US-Corporate/3M/US@3M-Corporate Deanna J. Luebker/US-Corporate/3M/US@3M-Corporate cc: Lisa A. Clem en/US-Corporate/3M /US@ 3M -Corporate Subject: T O X 145: PFOSA PK, Dose Verification Hi Andrew and Deanna: W e have completed our screen of the PFOSA dose in TWEEN. Error bars are about + /-3 0 % . PFOSA was determined in triplicate and PFOS and POAA from a single analysis. I'd classify this data as screening quality and if this data poses any major questions about the interpretation of the tox data, we may need more data points for the PFOS and POAA. However, I did check for the presence of the POAA on two different instruments. Also, in one of your voice mails, Andrew, you mentioned concern about photolysis of PFOSA to PFOS. All of the data that I've seen indicates that there may be photolysis of PFOSA to POAA (not verified yet), but there is no evidence of PFOSA photolysis to PFOS. Since the photolysis experiments were conducted under very strenuous conditions, I don't think you have much to worry about with your samples (at least not for a few dozen years!). In TWEEN 80: PFOSA 1 3 3 .2 6 % of expected dose of 1 0 0 0 //g /m L recovery 130% PFOS 1 85 % of expected dose of 10 //g/mL recovery 115% POAA recovery 121% --> 1330/;g/m L --> 18.5Ag/nnL ~ > 2 . 5 /yg/rnL spike spike spike Let me know if you have questions. kjh Andrew Seacat 10/27/99 02:53 PM 3M Medical Dept. Toxicology Services Andrew M. Seacat Ph.D. 3M Center 220-2E-02 Saint Paul, MN 5 5 1 44 Tel: (651) 575-3161 Fax: (6 5 1 )7 3 3 -1 7 7 3 To: Kris J. Hansen/US-Corporate/3M /US@ 3M -Corporate cc: Fred L. DeRoos/US-Corporate/3M/US@ 3M-Corporate Deanna J. Luebker/US-Corporate/3M/US@3M-Corporate Sue Chang/US-Corporate/3M/US@ 3M-Corporate Subject: PFOSA dosing solution Kris, As w e were discussing in our last Friday's meeting,we would like to have the PFOSA dosing solution checked for PFOSA concentration, and for PFOS and PFOA, which may under certain conditions arise from photolysis. W e left the dosing solution with you. I understand there is a problem with the Tween 80 concentraton being too high to allow sufficient dilution for analysis of some PFOS concentrations. Given that the starting material has approxmately 1% PFOS in it could the dosing solution sample be analysed to see if there is significantly more PFOS in there? If not possible, then perhaps we could ask Fred Deroos to analyze the dosing solution? The dosing solution was prepared as follows: Stock PFOSA in acetone was made up at 52mg PFOSA/O.52 mL acetone = 100 mg/mL This was diluted into 5 1 .4 8 ml of 2% Tween 80 to acheive the dosing solution: Final concentration of PFOSA = 1mg/ml Final cone of acetone = 1 % Final cone Tween 80 = "2% Thanks, Andrew TOX145 Tsveca 10- Doe Confinnilion Study Dale Analyzed F ile # Instrument Tween dose-NA TOXI45 11/2/99 110299a Soup 020199 Dose cone, (ppb) .^ ,, jE ip ecled Dose (ppb) Amt of spike (ppb) Dose + MS cone, (ppb) % Recovery o f Dose r isii) NA 20 4 29 48 VALUE! % Recovery o f MS Date of Extraction 121 11/2/99 if- -p \* ^ S) b l(A ff b 4 .V rf l O f f 4^ I* ' ^ po M A 2-4 fT*' 500 - 2 .< ? 0 n r - p )v\ L - 5" p ^ vy-L^ Study Date Analyzed File# Instrument . TOX145 10/29/99 102999a Soup 020199 PFOSA in 2% Tween 80, Sample TN-A-3046 File# 10299013 10299014 10299017 % Recovery of Dose Recovery of Dose amt (ppb) 132.64 265.27 134.31 268.62 132.83 265.65 Mean Standard Dev. % Rsn 133.26 0.917 0.688 1.83 0.688 p a r * - v `0< rr*' / t e c Tvvf**- ?foSA 3> (^ <tx^0 f ( / vxaJT^T 5 f< rW - PFOSA dosing solution ^ Andrew Seacat T : : 10/27/99 02:53 PM 3M Medical Dept. Toxicology Services Andrew M. Seacat Ph.D. 3M Center 220-2E-02 Saint Paul, MN 5 5 1 4 4 Tel: (6 5 1 )5 7 5 -3 1 6 1 Fax: (6 5 1 )7 3 3 -1 7 7 3 To: Kris J. Hansen/US-Corporate/3M/US@ 3M-Corporate cc: Fred L. DeRoos/US-Corporate/3M/US@ 3M-Corporate Deanna J. Luebker/US-Corporate/3M/US@3M-Corporate Sue Chang/US-Corporate/3M/US@3M-Corporate Subject: PFOSA dosing solution Kris, As we were discussing in our last Friday's meeting,we would like to have the PFOSA dosing solution checked for PFOSA concentration, and for PFOS and PFOA, which may under certain conditions arise from photolysis. We left the dosing solution with you. I understand there is a problem with the Tween 80 concentraton being too high to allow sufficient dilution for analysis of some PFOS concentrations. Given that the starting material has approxmately 1 % PFOS in it could the dosing solution sample be analysed to see if there is significantly more PFOS in there? If not possible, then perhaps we could ask Fred Deroos to analyze the dosing solution? The dosing solution was prepared as follows: Stock PFOSA in acetone was made up at 52mg PFOSA/O.52 mL acetone = 1 00 mg/mL This was diluted into 5 1 .4 8 ml of 2% Tween 8 0 to acheive the dosing solution: Final concentration of PFOSA = 1mg/ml Final cone of acetone = 1% Final cone Tween 8 0 = ~2% Thanks, Andrew Printed 11/04/99 /O M3 * -- -- * --------- [3M Restricted] Page 1 w /W * * *<1*1m l/ TOXI45 Tween IO- Do*e Canfinnilion S tu d y Date Analyzed File H Instru m e n t PO.AA Sam ple ID Tween dose-2ppb T O X I4 5 10/29/99 102999a Soup 020199 Dose cooc. (ppb) E ip ected Dose (ppb) Am t o f spike (ppb) D ose + MS cotte, (p % R ecovery o^DftJ'/ Recovery of M D ale of Extraction f y1 67 2 0 0 2 04 3 51 (*> 10/29/99 PFOS Sam ple ID Tween dose-2ppb Dose coac. (ppb) E ip ee te d D ose (ppb) A m t o f spike (ppb) D ose + M S conc. (p % R ecovery o f j?p % Recovery o ( M D a le o f E xtraction 4 13 200 2 07 6 40 f i 07 i_______Ui ) 10/29/99 Sam ple ID Tween dose-200ppb Dose conc. (ppb) Expected Dose (ppb) Am t of spike (ppb) Dose + M S conc. (p % Recovery 265 65 200 100 385 42 Recovery of M 1 120I ch |u W r.so b E c tim i /. 5 W <2 / x $ ^ ^ 9O ^ * ^[* < 0 ? 0 fr FA C T: DATA R E V IE W S L M M A K i H JK > i ^ " fa in j . a h ' Dale Dala Analyst: FACT Study * II 3s -To* r ts - Matrtx/Timepoir Sample List: / Set-up Analysis Date/Analyst: f,A i A f 3 ^ ? ___________________ __________ _ Instrument: ^ / `gg__________ ;---------------------------- Q Analyte: ~P^A A (C H l') Acceptable Linear Range: l O p j >l> > J o d jv L LOQ:__ / so j,ah---------- ra2: o - m / z / ______ Calibration Checks: ^ Extraction Blank: M'A Matrix Blank Ha -- t /> Jevtd*' MS/MSD:__________ __________ __________________________ Data Status: Analyte: 7/^^ <2> C C H ') Acceptable Linear Range: ! !)lj>j>L LOQ :____ ________________ J> ph Extracted Blank: V** D ata R eview Sign-O fT Analyst Review__ Name / Date: -AAs Technical Review . Name/ Date:___ _______ p j h l l / l Quality Assurance Review Name / Date:_____________________________ Data Entry:. Comments / Justifications: fU T S kjire -Ae/icdeef / ----------fix. Oxy-t/e /*- OrAfv }> A c*' u s Dn- J U . i^toey / t ~Ll L 'A F r CtA-C.- If a h-C f . k*e*>t*t- ^ a/lK- J bdvucs <V / r s i fLo.*. 0 ?7 g.--4 d e V fa -J /* n ~ z a r e v A t r * 7 ________^ * ~ > % -f* 4 L L U /e*' >* `^ S /; %/ S .t-c F C o.f u ''M.y' k /* -S A-o j cerf A-*- 5 U .' - 3 a * 'V o r/jtf <D Tu ^ /^ , R*2: a . f t t v r Calibration Checks: K- MS/MSD: Data Status: M atrix Blank: V fl 2 "f -f-*,' ~f-t &c c /u T c r /. 4U f u A r ,n f<, a ^ f h*" l/ajucs o-/ less- j AA D - g ^ c! /-/i> vud 4 U u F b o T L * 4 l laufetrf- < Z u rt-C Analyte: 7 ^ 5 ,* C c H 3 )w Acceptable Linear Range: LOQ: / a . } O r t , l /> h r> p l FF Extracted Blank:___ Ha CU-rV f p u f s . C o-H'tf U ns tC u frcJ -f / n , 7 ^ - /^Ca Us . --~ J S " L l f f t _____________________________ RA2: 0 -9i?Z ./ Calibration Checks: K- ~~~ MS/MSD: Data Satus: Matrix Blank: V A / duel- ~ i A -- f' / // / ro ffP fd U a r je r f AT fD fo (u 4l L t j J L r c * .x .c v ^ tA g W -f >o ytg rf /-3/y> X . f Dale Data Amlyjt; FACT Study X: Matnx/Timepoir Sample Last: Set-up Analysis Date/Analyst: FACT: DATA REVIEW SUMMARY FORM "Us Data Review Sign-OfT Analys1tReview t. 5 * * Name/ Date: ^ V w /ff rtfce' C j * - u io 7?fl p fn h i 5 Technical Review Name/ Date:___ i Quality Assurance Review Name/ Date:__________ Data Entry:. Instrument: W - 5>Z->/ ?? Analyte: X s S c fH ) AcceptableLinear Ranne: //A LOO AM RA2: N A Calibration Checks: Ha MS/MSD: Data Status: ExtractionBlank: A/M Matrix Blank: H A Com m ents / Ju stificatio n s: _________________________ <2) 6 ^ . ____________ J>awjh . < rttiX *_____ TC a~Yi lt- c < A - - S k - * J - f * C r f /H _ ^ X k S '' U l / t i . w X $X ) ftrfa. CovLnrk b't- t \ e . d U ^ L o u .I 4L ,* j L r tu - t.. L X X - f, C ^^ 6 - * - J A S ________________ f i u ) .S -- l T / C " _________ Q u a n tify Conpound Sunmary R eport TOX145-tween 80 dose confirmation for POAA, pros i POM* Sample List: C :\MASSLYNX\soup020199 .pro\SampleDB\102999a Last modified: Hethod: Fri Oct 29 10:23:59 1999 C : \MASSLYNX\soup020199.pro\MstbDB\102999* Last modified: MOD Nov 01 06:21:40 1999 Job Cods : Printed: Mon Nov 01 06:47:34 1999 10/29/99 las Confound 1: POAA (Chi) Nans 1 1G2999001 2 102999002 3 102999003 i 102999004 5 102999005 6 102999006 7 102999007 8 102999008 9 102999009 1C 102999010 11 102999011 12 102999012 13 102999013 14 102999014 15 102999015 1 102999016 17 102999017 18 102999018 19 102999019 20 102999020 21 102999021 22 102999022 23 102999023 24 102999024 25 102999025 26 102999026 27 102999027 28 102999028 29 102999029 Saaplelist Text MeOH Bile MeOH Bile FCMix-9908 6-43 -1, FCMix-99086-43- 2, FCMix-99086-43 -3. FCMix-99086-43 -4, FCMix-99086-43-5, FCMix-9 9086-4 3-6, FCMix-990 86-43-7. FCMix-990 86-43 -8, FCMix-99086'43 -9. Ippb- 9/10/99 RWW 5ppb- 9/10/99 RWW lOppb- 9/10/99 RWW 25ppb- 9/10/99 RWW 50ppb- 9/ 10/99 RWW lOOppc- 9/10/99 RWW 250ppc- 9/10/99 RWW 500ppb- 9/10/99 RWW 750ppb- 9/10/99 RWW MeOH BIX T C X145-PFOS/POAA in Tween-dose-2ppb- 10/29/99 IAS T O X 145-PFOS/POAA in Tween-os-4ppb- 10/29/99 IAS FCMix-9908 6-4 3-4 , 25ppb- 9/10/99 RWW TOX145-PFOSA in Tween-dose-200ppb- 10/29/99 IAS TCX145-PFOSA in Tween-ms-300ppb- 10/29/99 IAS FCMix-99086-43-7, 250ppb- 9/10/99 RWW MeOH BIX FCMix-99086-43-1, Ippb- 9/10/99 RWW FCMix-99086-4 3-2, 5ppb- 9/10/99 RWW FCMix-99086-43-3 , lOppb- 9/10/99 RWW FCMix-99086-43-4, 25ppb- 9/10/99 RWW FCMix-99086-43-5, 50ppb- 9/10/99 RWW FCMix-99086-43-6, lOOppb- 9/10/99 RWW FCMix-99 08 6-43-7, 2S0ppb- 9/10/99 RWW FCMix-99086-43-8, SOOppb- 9/10/99 RWW FCMix-990 86-43 -9. 750ppb- 9/10/99 RWW Typ Standard Standard Standard Standard Standard Standard Standard Standard Standard OC oc Standard Standard Standard Standard Standard Standard Standard Standard Standard Std Cone 1.00 5.02 10 . 00 25.10 50.20 100.00 251.00 502.00 752.00 25.10 251.00 1.00 5.02 10.00 25.10 50.20 100.00 251.00 502.00 752.0C RT 7.154 7.088 7.129 7.101 7.082 7.087 7.084 7.133 7.103 7.129 7.147 7.152 7.134 7.147 7.131 7.160 7.128 7.110 7.169 7.174 7.180 7.129 7.130 7.179 7.154 7.129 ,f/><In j '-U i 1 fp9 1 Area Flags 42 bb 16 MM S3 MM 108 bb 244 bb 471 bb 981 bb 2481 bbX 4254 bbX 5542 bbX 14 MM 22 MM 40 MM 259 bb 12 MM 11 MM 2363 bb 13 MM 67 MM 113 MM 273 MM 542 bb 1024 MM 2338 bbX 4210 bbX 5411 bbX Cone. *Dev 3.66 i.o : 4.72 10.22 23.74 46.43 97.28 246.70 423.45 551.77 0.92 1.67 3 .51 25.32 2 -6 2 -5 -8 -3 -2 -16 -27 1 0.70 0.61 234.97 -6 0.73 6.15 10.72 26.64 53.45 101.52 232.52 418.97 538.72 -27 23 7 6 6 2 -7 -17 -28 Soup 020199: Quantitated and printad by las on 11/01/99 Q u a n tify Compound S u n n ary M p o r t XOX145-tween 80 dose confirmation for POAA, PFOS, k POAA- xt 10/29/99 le* Semple List: Lese modified: Method: Lest modified: Job Code: C :\H X S S L Y N X \sou p 020199.p ro\8eap leD B M 02999e Pri Oct 29 10:23:59 1999 C: \MASSL\soup020199 .pro\MethDB\102999e M on N ov 01 06:21:40 1999 Printed: Mon Nov 01 06:47:34 1999 Compound 2: PPOS (Ch2) f Nana 1 102999001 ; 102999002 3 102999003 4 102999004 5 102999005 1C2999006 - 1C29990C7 e 1029990CS 9 102999009 10 :::9990io 13 102999011 11 102999012 13 102999013 14 102999014 15 102999015 16 102999016 17 102999017 13 102999018 19 102999019 20 102999020 21 102999021 22 102999022 23 102999023 2; 102999024 25 102999025 26 102999026 27 102999027 2 3 102999028 29 102999029 Samplelist Text MeOH Blk MeOH Blk FCMix-99086-43-1 FCMix-990 86 -43-2 FCMix-99 086-43 -3 lppb- 9/10/99 RWW 5ppb- 9/10/99 RWW lOppb- 9.10/99 RWW FCMix-990 86-4 3-4 FCMix-99 086-4 3-5 FCMix-990 86-4 3-o FCMix-99086-43-7 FCMix-9903 6-4 3-8 FCMix-990 86-43-9 25ppb- 9/10/99 RWW SOppb- 9/10/99 RWW lOOppb- 9/10/99 RWW 250ppb- 9/10/99 RWW 500ppb- 9/10/99 RWW 7 SOppb- 9/10/99 RWW MeOH Blk TOX145-PFOS/POAA in Tween-dose-2ppb- 10/29/99 IAS TOX14S-PFOS/POAA in Tween-ms-4ppb- 10/29/99 IAS FCMix-99086-43-4 . 25ppb- 9/10/99 RWW MeOH Blk TOX145-PFOSA in Tween-dose-200ppb- 10/29/99 IAS TOX145-PFOSA in Tween-ms-3OOppb- 10/29/99 IAS FCMix-990 86-43 -7, 250ppb- 9/10/99 RWW MeOH Blk FCMix-990 86-43 -1 , lppb- 9/10/99 RWW FCMix-9908 6-43-2 , Sppb- 9/10/99 RWW FCMix-990 86-43 -3 , lOppb- 9/10/99 RWW FCMix-99086-43-4 , 25ppb- 9/10/99 RWW FCMix-99086-43-5 , SOppb- 9/10/99 RWW FCMix-9908 6-4 3-6 , lOOppb- 9/10/99 RWW FCMix-9908 6-43-7 . 2SOppb- 9/10/99 RWW FCMix-99086-4 3-8 . SOOppb- 9/10/99 RWW FCMix-99086-43-9 , 750ppb- 9/10/99 RWW Type Standard Standard Standard Standard Standard Standard Standard Standard Standard QC QC Standard Standard Standard Standard Standard Standard Standard Standard Standard Std Cone 1.01 S 03 10.00 25.20 50.30 101.00 252.00 503.00 7S5.0G 25..20 252..00 1 ..01 5 .03 10..00 25..20 50..30 101..00 252..00 503..00 755 .00 RT 7.315 7.295 7.226 7.291 7.240 7.266 7.249 7.246 7.272 7.265 7.289 7.309 7.313 7.340 7.331 7.338 7.314 7.321 7.313 7.295 7.272 7.330 7.335 7.342 7.291 7.313 7.363 7.314 7.291 Area Flags 202 bb 42 bb 148 MM 476 MM 913 MM 2108 bb 4162 bd 8473 bd 22878 bbX 41708 bbX 56477 bbX 170 MM 424 bb 619 bb 2284 bb 63 MM 373 MM 398 MM 22863 bb 91 bb 158 bb 530 bb 989 bb 2289 bb 4761 bb 8949 bb 22364 bbX 42068 bbX 55588 bbX Cone. *Dev 1.56 0.00 0.93 -8 4.74 -6 9.81 23.71 -2 -6 47.57 -5 97.67 -3 265.05 5 4S3-87 -4 655.48 -13 1.18 4.13 6.40 25.75 2 0 .OC 3.55 3 .83 264.88 0.27 5 1.04 3 5.37 7 10.70 7 25.80 2 54.53 8 103.19 2 259.08 488.05 -3 645.14 -15 Page 2 Soup 020199: Quantitated and printed b y las on 11/01/99 Q u a n tify Compound Sunitary R ep o rt TOX145-twaen 80 dose confirmation for POAA, PROS k FOAA- ext 10/ 29/99 ia s Sample List: Lese modified: Method: Last modified: Job Code : C: \MASSLYNX\soup02 0199.pro\Saa*>leDB\102999a Tri Oct 29 10:23:59 1999 020199 102999C :\K A S S L Y N X \S O U p .p rO \M e th O B \ 01 06 21:40 1999Mon Nov : a Printed: Mon Nov 01 06:47:34 1999 compound 3: p ro s a <ch3) Name 1 102999001 2 102999002 i 102999003 102999004 c 1029990C5 102999006 - 102999007 8 10299900S 9 102999009 1C299901C 102999011 22 102999012 102999013 2- 102999014 15 102999015 I d 1 0 : 999016 17 10 999017 13 102 9990 IS 19 102 999019 20 102999020 21 102999021 22 102999022 23 102999023 24 102 999 024 25 102999025 26 102999026 102999027 23 102999028 29 1C2999029 Samplelist Text MeOH BIX MeOH BIX FCMix-9908 6-43 -1. lppb- 9/10/99 RWW FCMix-99086-43 -2, 5ppb- 9.10/99 RWW FCMix-99086 -43-3. lOppb- 9/10/99 RWW FCMix-99086-43-4, 25ppb- 9/10/99 RWW FCMix-99086-43-5, 50ppb- 9/10/99 RWW FCMix-990 86-4 3-6, lOOppb- 9/10/99 RWW FCMix-990 86-4 3-7, 250ppb- 9/10/99 RWW FCMix-9908o-43-8, SOOppb- 9/10/99 RWW FCMix-9 90 86-4 3-9. 75Oppb- 9/10/99 RWW MeOH BIX TCX145 -PFOS/POAA in Tween-dose-2ppb- 10/29/99 IAS TCX145-PFOS/POAA ir. Tween-as-4ppb- 10 9 IAS FCMix-99086- 43 -4, 25ppb- 9/10/99 RWW MeOH BIX TCX14S-PF0SA in Tween-dose-200ppb- 10/29/99 IAS TOX14 S-PFOSA in Tween-ms -3OQppb- 10/29/99 IAS FCMix-990 86-43 - 7. 2S0ppb- 9/10/99 RWW MeOH BIX FCMix-99086-43 -1, lppb- 9/10/99 RWW FCMix-99086-43-2, 5ppb- 9/10/99 RWW FCMix-99086 -43-3, lOppb- 9/10/99 RWW FCM ix-99086-43-4. 25ppb- 9/10/99 RWW FCMix-99086-43-5. 5Qppb- 9/10/99 RWW FCMix-99086-43-6. lOOppb- 9/10/99 RWW FCMix-99086-43-7, 250ppb- 9/10/99 RWW FCMix-990 86-4 3-8, SOOppb- 9/10/99 RWW FCMix-990 B6-43 -9. 75ppc- 9/10/99 RWW 0 0 Typ Standard Standard Standard Standard Standard Standard Standard Standard Standard QC Standard Standard Standard Standard Standard Standard Standard Standard Standard Std Cone 1.01 5.03 10.10 25.10 50.30 101.00 251.00 503.00 754.0C 25.10 251.00 1.01 5.03 10.10 25.10 50.30 101.00 251.00 503.00 754.00 RT 7.833 7.79C 7.741 7.809 7.803 7.805 7.766 7.809 7.857 7.895 7.941 7.982 7.92G 7.969 7.984 7.989 7.943 7.950 7.964 7.990 7.947 8.003 7.988 7.948 7 .942 7.965 7.992 7.989 7.917 Area Flaps 18209 MM 835 MM 1102 MMX 1881 MMX 2710 MM 6408 MM 10741 MM 21634 MM 68915 MM 139095 MM 199487 MM 2140 MM 72407 bb 73318 bb 8797 MM 596 MM 72510 bd 105109 db 75327 MM 870 MM 783 MMX 1994 MMX 3433 MM 8204 MM 14786 MM 30309 MM 76993 MM 140797 MM 201774 MM Cone. XDev 66.15 2.32 3.30 227 6.16 23 9.21 22.80 -9 _Q 38.71 -2 3 78.74 -22 252.44 1 510.22 1 732.15 -3 7.12 265.27 268.62 31.57 26 1.44 265.65 38S.42 276.00 1C 2.45 2 .13 111 6.S8 31 11.87 17 29.39 17 53 .58 7 110.61 10 282.14 12 516.53 3 740.56 -2 Pape 3 Soup 020199: Quantitated and printed by ias on 11/01/99 Q u a n tify Compound S u n n ary R ap o rt TOX14S-tw*an 80 dosa confirmation for POAA, Pros k POAA- Sarapla List: Last modified: Method: Last nodifiad: Job Coda: C \MASSLYNX\soup020199 .p ro \San>laDB\ 102999a Fri Oct 29 10:23:59 1999 4,,,,a C : \ M A S S L YMX\soup020199.pro\MethDB\102999a Mon Nov 01 06:21:40 1999 Printed: Non Nov 01 06:47:34 1999 10/29/99 l a s Compound 4: IS (Ch4) e Nane 1 1029990 Gl 2 102999002 3 102999003 4 1C2999004 5 102999CC5 lG299900o -, 132999C3" 0 102999003 G 1Q29990C9 IC 2999010 102999C11 12 102999012 13 102999013 li 102999014 15 102999015 io 102999016 2_- 102999017 18 102999018 19 102999019 20 102999020 21 102999021 22 102999022 23 102999023 24 102999024 25 102999025 26 102999026 2? 10299902" 23 102999C2S 29 102999029 Saaplelist Text MeOH BIX MeOH BIX FCMix-99086-43-1. Ippb- 9/10/99 RWW FCMix-990 86-4 3-2. 5ppb- 9/10/99 RWW FCMix-990 86 -43-3, lOppb- 9/10/99 RWW FCMix-99086 -43- 4, 25ppb- 9/10/99 RWW FCMix-9 908 6-4 3-5. SOppb- 9/10/99 RWW FCMix-99 086 -43-6. lOOppb- 9/10/99 RWW FCMix-990 86 -43-7, 2SOppb- 9/10/99 RWW FCMix-99086 -43 -S, 500ppb- 9/10/99 RWW FCMix-9 908 6-43-9. 7 SOppb- 9/10/99 RWW MeOH BIX TOX145-PFOS/POAA in Tween-dose-2ppb- 10/29/99 IAS TOX145-PFOS/POAA in Tween-ms-4ppb- 10/29/99 IAS FCMix-99086-43 -4 , 2 Sppb- 9/10/99 RWW MeOH BIX TOX145-PFOSA in TTween-dose-200ppb- 10/29/99 IAS TOX145-PFOSA in TTween-ms-3OOppb- 10/29/99 IAS FCMix-990 86-4 3-7, 250ppb- 9/10/99 RWW MeOH BIX FCMix-99086-43-1, Ippb- 9/10/99 RWW FCMix-9908 6-4 3-2, 5ppb- 9/10/99 RWW FCMix-9908 6-43 -3. lOppb- 9/10/99 RWW FCMix-99 086-43-4, 2 5ppb- 9/10/99 RWW FCMix-99086-43-5, SOppb- 9/10/99 RWW FCMix-990 86-43 -6, lOOppb- 9/10/99 RWW FCMix-9908 6-43-7, 250ppb- 9/10/99 RWW FCMix-9908 6-4 3-8, SOOppb- 9/10/99 RWW FCMix-990 86 -43- 9, 750ppb- 9/10/99 RWW Type Standard Standard Standard Standard Standard Standard Standard Standard Standard OC OC Standard Standard Standard Standard Standard Standard Standard Standard Standard 6td Conc 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.0C 1.00 1.00 1.00 1.00 1.00 1.00 1.00 RT 7.170 7.082 7.147 7.095 7.099 7.104 7.101 7.128 7.120 7.145 7.169 7.150 7.163 7.147 7.154 7.146 7.127 7.163 7.168 7.174 7.145 7.147 7.174 7.146 7.146 Area Plaga 15 bb 4292 bb 4289 bb 4424 bb 4486 bb 4446 bb 4093 bb 2630 bb 1993 bb 1842 bb 2613 bb 1041 bb 2305 bb 2529 bb 1016 bb 1991 bb 2320 bb 2361 bb 2396 bb 2274 bb 2435 bb 2181 bb 2059 bb 1934 bb 1818 bb Conc. HD0V 0.01 -95 1.48 1.48 1. 52 1.54 1.53 1.41 0 .91 0.69 0.63 48 48 52 54 53 41 -9 -31 -37 0.90 -10 0.36 -64 0 .79 -21 0.87 0.35 0.69 -13 -65 -31 0.80 0.81 0.83 0.78 0.84 0.75 0.71 0.67 0.63 -20 -19 -17 -22 -16 -25 -29 -33 -37 Paga 4 Soup 020199: Quantitated and printed by ias on 11/01/99 M ethod R e po rt Method file: Last modifiedCompound Printed: CC::\\MMAASbSLStLfNYiN)X\soupQ20199.pro\MethDB\102999a.mdb MMoonn NNoovv 0011 06:21:40 1999 1:: POAA (Chtil'l;: Mon Nov 01 07:36:09 1999 Compound Name: Internal Ref.; Quantify Trace: Cone, of Standards: User RF Value: User Peak Factor: Integrate Window Factor; Chromatogram mass window: POAA (Chi: (None] TIC Cone. A 1.000000, Disabled 1.000000 2.000 l.OOOODa Retention Time (mins): Relative Retention Time: RT Reference; Time Window (mms) ; Peak Selection: 7.173, Enabled 0.000, Disabled (None] 0.312 Nearest Response Type; Response: External Areas Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Linear Exclude 1/X None Units: Peak-to-peak amplitude: Smoothing: Window size (scans): Number of smooths: Smoothing method: Join valley threshold: Reduce peak tailing: Raise baseline maximum: Draw vertical threshold: Detect shoulders: Shoulder threshold: Relative height: Absolute height: Relative area: Absolute area: 90 Enabled 1 30.00 200.00 5.00 90.00 Disabled 30.00 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled Page 1 M ethod R e po rt Method file: Last modified: Compound: Printed: C:\MASSLYNX\soup020199.pro\MethDB\102999a.mdb Mon Nov 01 06:21:40 1999 2; PFOS (Ch2 : Mon Nov 01 07:36:09 1999 Compound Name: Internal Ref.: Quantify Trace; Cone, of Standards; User RF Value: User Peak Factor: Integrate Window Factor: Chromatogram mass window: PFOS (Ch2) [None! TIC Cone. B 1.000000, Disabled 1.000000 2.000 1.QOOODa Retention Time ;mins;: Relative Retention Time: RT Reference; Time Window :mms: : Peak Selection: 7.434. Enabled 0.000, Disabled [None 1 0.345 Nearest Response Type: Response: External Areas Polynomial Type: Point of Origin: Fit weighting: Axis Transformation: Linear Exclude 1/X None Units: Peak-to-peak amplitude: Smootning; Window size (scans ; Number of smooths: Smoothing method: Join valley threshold: Reduce peak tailing; Raise baseline maximum: Draw vertical threshold: Detect shoulders. Shoulder threshold: Relative height: Absolute height: Relative area: Absolute area: 83 Enabled 30 .00 200.00 5.00 90.00 Disabled 30.00 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled Quantify Calibration Report ia/29/99 las T O X U S - t -- n 60 do., confirmation for POX*, p r o s , i POAA- t . 10/29/99 U > Compound 1 name: POAA (Ch1) Coefficient of Determination: 0.997121 Calibration curve: 10.0347 * x + 5.23213 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans. None 7.55e3-i X U u/*> hr Mi f Page 1 Soup 020199: Quantitated and printed by laa on 11/01/99 Quantify Calibration Raport TOX145-twn 80 doaa confirmation for POAA, PF06, * 10/29/99 las ICompound 2 name: PFO S (Ch2) Coefficient of Determination: 0.996935 Calibration curve: 8 6.0577 ' x + 68.0228 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None Pag 2 Soup 020199: Quantitatad and printad by las on 11/01/99 Quantify Calibration Haport I O X K S - w m i i 80 dosa confirmation for PQAA, P ro s t POAA- axt. 10/29/99 iaa (Compound 3 name: PFOSA (Ch3) (Coefficient of Determination: 0.997261 Calibration curve: 2 72.189 ' x + 203.159 (Response type: External Std, Area (Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None Soup 020199: Quantitatad and printed by las on 11/01/99 Quantify Calibration Mport XOX145-tween 80 dosa confiziaation for POAA, "OS. t POAA- xc. 10/29/99 l u Compound 4 name: IS (Ch4) Response Factor: 2904.16 Response type: External Std, Area Curve type: RF 4.49e3-> Pag* 4 X vX x Soup 020199: Quantitatad and printad by iaa on 11/01/99 Laboratory Report Analytical Report of Data for PFOSA Pharmacokinetic Study in Rats (Sera and Liver) Laboratory Report No. FACT-TOX-145 (W2814) Requester Project No. T-7132.2 Attachment E Extraction and Analytical Data Extraction Worksheet ETS-8-6.0 Study # T t ix - H J ~ _______ Surrogate Std Matrix'i f l . t L ', J o - Approx, ppm Box # jfc `H -2 -O Q ___ Actual ppm WK/Dav 1* y DateSpiked/Analyst ,n - t i - r r / s ^ RBL10139-250ppD-CCV-11-1 104 5 uL 9R03230M.Dy1 Control-250ppb-MS/D11 5 uL 9R03235M,Dy4.Control.250pDb-MS/D12 5 uL FC Mix FC Mix FC Mix approx.0.5 ppm approx.5 ppm approx.50 ppm actual ppm actual ppm actual ppm # 9 `io6 (.-V 7-2 # 9 *o ft, <4 )-l 11 tQ < /Lr/ ?10 uL - - 10 uL - - 10 uL - Comments Verified By - A)/Ft____ RBL10139-H2O blk-11&12 RBL10139-Liver blk-11&12 RBL10139-5pDb-11&12 RBL10139-10ppb-11&12 RBL10139-25ppb-11&12 RBL10139-50ppb-11&12 RBL10l39-100ppb-11&12 RBL10139-250ppb-11&12 RBL10139-500ppb-11412 RBL10139-750ppt>-11&12 RBL10139-1000ppb-11&12 9R03230M,Dy1.Control 9R03231M.Dy1,Control 9R03232M.Dy1.Control 9R 03233M .D y1.C o ntrol 9R Q 32 34M ,D y1.C o n tro l 9R 03245M ,D y1.5m g /kg 9R 03246M .D y1,5m g yk g 9R 03247M .D y1,5m g/kg 9R 03248M .D y1.5m g/kg 9R03249M .Dyl.5m g/kg 9R 03235M ,D y4,C o n tro l 9R 03236M ,D y4.C o n tro l 9R 03237M ,D y4.C o n tro l 9R 03238M ,D y4.C o n tro l Blank-TLahto. U.'w Liver Extraction Method 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 2 uL 4 uL 10 uL 20 uL 40 uL - 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL Std# W o H s / i S* ETS-8-6.0 10 uL 20 uL 30 uL amount = l o 4 uL - i' ml n / C , 1 g/ml Date & initials SrtL io le __ HI_a____ Vortex 15 Sec. lo -ia Pipette Matrix, spike with appropriate surrogate or FC-Mix Volume / O ml Pipette 1 ml of 0.5 M TBA, pH 10. pH= l u /t / J - f f A , -- Std. # M O i O '/ J - i c , Pipette 2 ml of 0.25 M Na,CO3/0.25 M NaHCO, buffer Std. # HHoiL- `l/ - o g \L____ u u a foliar Dispense 5 ml of methyl-t-butyl ether Shake 20 min Centrifuge 20-25 min. TN -A -^V v Shaker speed: Centrifuqe speed: 3 TO'-/ ___ / M l/I____ Remove a 4 ml aliquat of organic layer / Put on Nitrogen Evaporator to dryness Temperature: Room Temo. Add methanol Volume / ml TN-A- O U T Vortex 30 sec / Filter using a 3cc B-D syringe with a 0.2 um filter into an autosampler vial <// v ' ftv - 1 ' U e s i - C J l S u y r o A i i . ^ ( i I / w a 3 .n t . o ( (c o o rpb *ri uoo-o a<id fir ^ri<- ^ T f y i - b Mwi aJujHtr O e (^ o n :o I c u ^ c . ^ - . i vi, u t 1 0 0 0 ^ , - 1 , , o ( . S - k .^ e x v ' . `- * ' -H < b ^ _ . , o - / 3 - ' < A K / 10/12/99 Draft Attachment A ETS-8-6.0 Extraction of PFOS from Liver Form Comgpllpgtiioon / Verified By M ~ - W l Extraction Worksheet ETS-8-6.0 10/12/99 Draft Attachment A ETS-8-6.0 Extraction of PFOS from Liver Form Comi Verified By Sample Weights/ Volumes " V ln W Prep Date(s): 10-12-99 Analyst(s): SEE Sample Matrix: Rat Liver Mcthod/Revision: ETS-8-6.0 Target Analyte(s): PFOS, PFOSA Sample ID 9R03230M.Dyl.Control 9R0323IM.Dyl,Control 9R03232M ,D yl. Control 9R03233M,Dyl,Control 9R03234M.Dyl,Control 9R03245M,Dyl,5mg/kg 9R03246M.Dy 1,5mg/kg 9R03247M,Dy 1,5mg/kg 9R03248M,Dyl,5mg/kg 9R03249M.Dy 1,5mg/kg 9R03235M,Dy4,Control 9R03236M,Dy4,Control 9R03237M.Dy4 .Control 9R03238M,Dy4.Control 9R03239M,Dy4,Control 9R03250M,Dy4,5mg/kg 9R03251M.Dy4,5mg/kg 9R03252M,Dy4,5mg/kg 9R03253M.Dy4.5mg/kg 9R03254M.Dy4.5mg/kg Study Number: TOX-145 Equipment Number: 0222-0900 Final Solvent & TN Number: MeOH / TN-A-2945 Matrix Blank/Identifier: Rabbit Liver Box: 99-200 Initial Weight grams Homogenized By: Verified By: Comments U sed for M S/D 11 i.o in / . OOOO 09918 _ 1 ___________ ________________________ ____ ______ __________ i ____________ A )/A t.ljn i-o m I.OOTV /.o le 1.011,1 0.9119 1. OOl i j M M t M illa s . t\) a __________ U sed for M S /D 12 /. / . oo*<4 ___ o . I l o r l.oi 1/ ____________ m * _______________ ____________ J L _______________ A / . OOT. 1 .0 0 X 1 o .n n b ' o u i ______ -i-y J-/3 f i Summary of method: Notes: Review Date Rtl 10139 Form Approved by/Date:________________________ Form Com pletiot^v / ./ . Verified By: Id ton Pau Standard C u rv e s-T ilm o Prep Del*): HVI A aelysM t): Sample M ains: SEE R.u Liver M rlbod/Revisw n: ETS-8-fi o T arget Aaalylet!: Fc-Mix Bos Number: 99-200 FC M is Std Appros. 0 500 ppm: FC M is Std A p prt. 5 00 ppm: FC M is Std Appros. 50 0 ppm: Surrogate Std Appros. 100 ppm: *086-47.; 086-47-1 095-33 99086-13-11 Study Number: TOX-145 Equipment Number: 0222-0900 Final Solvent A TN Number: MeOK-TN-A-2945 Blank Tiwue/ldentirier: Rabbit L tver9086-13-5 Blank liver initial density (g) for cu rv o : Final otveal volume |n L ) for curves: 0 163 1000 PFOS 0 5000 0 5000 0 5000 5 000 5000 50 00 PFOSA Std Conc ug/mL 0 5005 0 5050 0 5050 0 5050 0 5050 5 005 5 005 5005 50 05 PFOSEA Sld Conc ug/mL 0 4997 0 4997 0 4997 0 4997 0 4997 4 997 4 997 4 997 49 97 PFOSAA Std Conc ug/mL 0 4999 0 4999 0 4999 0 4999 0 4999 4 999 4 999 4 999 49 99 EtFOSE-OH Std Conc ug/mL 0 5005 0 5005 0 5005 0 5005 0 5005 5 005 5 005 5005 50 05 MS56 Std Conc ug/mL 0 5010 0 5010 05010 0 5010 0 5010 5010 5010 5010 50 10 AH A m i Spiked mL 0 002 0004 0010 0 020 0 040 0010 0 020 0030 0004 Density 8 0 163 0 163 0 163 0 163 0 163 0 163 0 163 0.163 0 163 Calculated Concentrations o f Standards in the sample macnx ' PFOS PFOSA PFOSEA PFOSAA Std Conc Std Conc. Std Conc 6 !4 ng/g ng/g 6 13 6.13 30 7 307 613 920 1227 124 31 0 62 0 307 614 921 1228 12.3 30 7 61 3 123 307 613 920 1226 12.3 30 7 61 3 123 307 613 920 1227 PFOS Final Conc ng/mL 2.00 5 00 50 0 100 150 200 PFOSA Final Conc ng/mL l 00 2 02 5 05 10 1 20 2 50 1 100 150 200 the 1 0 mL final solvent volume PFOSEA PFOSAA Final Conc. Final Conc ng/mL 100 ng/mL 1 00 20 0 2.00 500 5.00 100 100 20 0 20 0 50 0 50 0 100 100 150 150 200 200 EtFOSE-OH Std Conc "8*8_______ 6.14 12.3 30 7 61 4 123 307 614 921 1228 ........... EtFOSE-OH Final Conc ng/mL 100 200 501 100 20 0 50 1 100 150 200 M556 Surrogate Std Conc Std Conc. " 8 ______ 6.15 ug/mL 100 12.3 Surrogate 30 7 Final Conc. 61 5 _______ 588_______ 123 3077 307 615 922 1229 Ad A m i Spiked mL 0 005 M5S6 Std Conc. ng/mL 1 00 200 501 100 200 50 ! 100 150 200 Surrogate Std Conc. ug/mL too Surrogate Final Conc ng/mL 502 AU A m i Spiked mL 0 005 Sample used for MS/MSD' 9R 03230M ,D yl Control PFOS Final Conc. ng/g 301 30! PFOSA Final Conc. TiV% 30! 301 PFOSEA Final Conc "S'! 301 301 PFOSAA Final Conc 8/8 ' 301 301 Initial Volume (mL)' S 00 EtFOSE-OH MSS6 Final Conc Std Conc. "8/8 n*/g 301 302 30! 302 Approx. Std Cone.. S.00 ug/mL A m i Spiked (mL) Density 0 010 0 166 Sample used for MS/MSD 03230M . D y! Control MS/MSD calc Insolvent PFOS PFOSA PFOSEA Final Cone Final Conc Final Conc. "H/H 50 0 ng/g 50 1 ng/g 50 0 50 0 SO i 50 0 PFOSAA Final Conc "IPS 50 0 50 0 Initial Volume (mL) 5 00 EtFOSE-OH M556 Final Conc Std Conc "8/8 50 1 g/g 50 1 50 l 50 1 Approx. Std Cone S 00 ug/mL A m i Spiked (mL) 0010 Final Vol 1000 Sim ple used for MS/MSD 9R03235M . Dy4. control MS/MSD calc. In matrix Initial W u g ) 1001 PFOS PFOSA PFOSEA Final Conc Final Conc Final Conc ng/g ng/g ng/g 301 30! 301 301 301 301 PFOSAA Final Conc "8/S 301 30! Initial Volume (mL) 5 00 EtFOSE-OH M556 Final Conc Sld Conc Appro Sld Cone 5 00 og/mL Am t Spiked (mL) Density "S'! "8/8______ 301 302 30) 302 Sample used for MS/MSD 03235M . Dy4. control MS/MSD calc Insolvent Initial Wt ig) 1001 PFOS PFOSA PFOSEA Final Conc Final Conc Final Conc n gg "S'* n*>* 50 0 50 1 50 0 50 0 50 1 50 0 PFOSAA Final Conc "/ 50 0 50 0 Initial Volume <mL) 5 00 EtFOSE-OH M5S6 Final Conc Std Conc "8/8 50 1 50 1 "8/8 50 1 50 l Approx Std Cone S 00 ug/mL A m i Spiked (mL) Final Vol 0010 1 000 * All Voi mL I 000 I000 1000 I000 I 000 I 000 1000 I 000 1.000 " HI i f lo-iH -1< Ion Pair Std Extraction Sheet ywrvh>*J <v\H/o ^ DILUTIONS SUMMARY SHEET MiMAr lOjlo HStudy: T O X -045 D ilution D ate/A nalyst: M C H 10/18/99 .l f tqq B ox #: 99-200 sample number or descrpilion 1:100 1: 1: 1: 9R03237M. Day 4, Control (3 if 9R032\5M . Day 1,5 mg/kg Dl 00 Dl 00 9R03246M. Day 1, 5 mg/kg 9R03247M. Day 1,5 mg/kg Dl 00 Dl 00 9R03248M. Day 1, 5 mg/kg 9R03249M, Day 1,5 mg/kg 9R0325IM. Day 4, 5 mg/kg Dl 00 D l 00 Dl 00 / 9R03252M, Day 4, 5 mg/kg 9R03253M. Day 4, 5 mg/kg 9R03254M, Day 4, 5 mg/kg Dl 00 Dl 00 Dl 00 SoIventATN N um ber: J l^ O H T M ' E xtraction D ate/A nalyst: SE E , 10/13/99 M atrix/T im epoint: Rat Liver /UA/Ur DILUTIONS 1: 1: 1: /y / Comments Verified By KJyv / SUM idit M n w l * ____ lo ( Ci 11 5 iu/ kv UlU /0|( (11 L______ .. _J._________ -A / _____ \ / I**** I )lirlw Notes: DIOO=IO uL sample + 990 uL MeOH. SMjAr 2 Form Completion Verified By: to Extraction Worksheet ETS-8-4.1 Studv # "p -,x H r Matrix "7. a t S. - Box # A Q - J i l -----------------WK/Dav rt- I'M DateSpiked/Analyst RBS10199-250ppt>-CCV-11-1 to 4 RTS 10199-250ppb-MS/D-11 RTS10199-Serum Blank-11412 RBS10199-H2O blk-11&12 RBS10199-Serum blk-11&12 RBS10199-5ppb-11&12 RBS10199-10ppb-11&12 Surrogate Std Approx, ppm Actual ppm #Mcic-i, O n i e - t r>-v9 /S o '5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL FC Mix FC Mix approx.0.5 ppm approx.5 ppm actual ppm actual ppm # 991. L V i- 11-1 lu-> V - W 10 uL 20 uL - FC Mix approx.50 ppm actual ppm U 99C 9S-13 lu -l-l-V t/jQ ----5L 5 uL ` - Comments Verified By _____ _J1 rt- RBS10199-25ppb-11&12 5 uL - 5 uL RBS10199-50ppb-11&12 5 uL - 10 uL ' RBS10199-100ppb-11&12 5 uL - 20 uL - RBS10199-250ppb-11&12 RBS10199-500ppb-11&12 RBS10199-750ppb-11&12 RBS10199-1000ppb-11&12 5 uL 5 uL 5 uL 5 uL - - 5 uL - 10 uL - 15 uL - 20 uL 9R03230M,Dy1 .Control 5 uL - - - 9R03231M,Dy1,Control 5 uL - - 9R03232M,Dy1 .Control 5 uL - - - 9R03233M,Dy1,Control 5 uL - - 9R03234M.Dy1 .Control 5 uL - - 9R03245M,Dy1,5mg/kg 5 uL - - 9R03246M.Dy1.5mg/kg 5 uL - - - / i w i o N *^ -- e *-- -- \ --------- 9R03247M,Dy1,5mg/kg 9R03248M,Dy1,5mg/kg 9R03249M,Dy1,5mg/kg 9R03235M,Dy4,Control 9R03236M,Dy4,Control 9R03237M.Dy4,Control 9R03238M,Dy4,Conirol 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL - -- - * * - V Blank-Tt oioWLy W u - Std# q q o c .a -s h amount = i- O ml------- Serum Extraction Method ETS-8-4J : Date & ,nitials = J ______ Vortex 15 Sec. Pipette Matrix, spike with appropriate surrogate or FC-Mix Volume 1 - 0 _.ml ' Pipette 1 ml of 0.5 MTBA, pH 10. pH= i o - IC tfl')/9 9 Std. # MMOiO - / v i e JlJirlOlMK! Pipette 2 ml of 0.25 M NajCOj/0.25 M N aH C 03 buffer Dispense 5 ml of methyl-t-butyl ether Std. # 9 Q OiW.cticATN-A- 3 9 9 (? = J ______ Shake 20 min Centrifuqe 20-25 min. Remove a 4 ml aliquat of organic layer Put on Nitroqen Evaporator to dryness Shaker SDeed: 3 0 0 Centnfuae speed: 3 VD<J Temperature. R o o m T em p . = m ____ vi* M im ic i'' AHH mAthannl Volume A_L2_ TN-A-3>VVi Vortex 30 sec. Filter usino a 3cc B-D svrinqe with a 0.2 urn filter into an autosampler vial Cont. Cal. Verifications used same matrix as for std curve. (u>, 10 \c<q S-*-' 0 r\hiv\ roJt W "n TVv. r o i ^^ m iomM'' \ lOlh ' U m !(?!&, (o - it - t 'l -- - 10/12/99 Draft Attachment A ETS-8-4.1 Extraction of PFOS from Serum Form Completion , / Verified Bv HIM Extraction Worksheet ETS-8-4.1 Study # -ft,;* Matrix ~i.ij 1 W u Rnx # <Ki _______ Date'Spiked/Analyst 9R03239M.Dy4,Control 9R03250M,Dy4,5mg/kg 9R03251M.Dy4,5mg/kg 9R03252M.Dy4,5mg/kg 9R03253M.Dy4.5mg/kg 9R03254M,Dy4,5mg/kg Surrogate Std Approx, ppm Actual ppm # 11 m -t <j- 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL - FC Mix FC Mix FC Mix approx.0.5 ppm approx.5 ppm approx.50 ppm actual ppm actual ppm actual ppm r-'V * (V| 1------- #----r--oHr*--------- - ---------- ---------7 .- ' Comments Verified By M/ fir Ni M -------_ J ---------- -4 -- - 4 ---------- -/ - - -z' - -- ______ ' . - -s ./ - * - ) S ' 1/ * - .- - - -* - --- ------------------ -- 7 ^ - -----------^ -------------------- 7---------------- ------------------------- ------------ ^ - --------------------- ^7 ^ - -- : . . . . . B l a n k V m _____ Std# qqoc,: -v? Serum Extraction Method__ ETS-8-4.1 - - - - -- - amount = / O * - ' / ______ Date & Ir itial 5 Vortex 15 Sec. ___________________________ PiDette Matrix, spike with appropriate surrogate or FC-Mix Volume----- / O ml___________ -- Pipette 1 ml of 0.5 M TBA, pH 10. pH= in / o - i f - v ' / * - Std.# W o ti,- / i;lJc. Pipette 2 ml of 0.25 M Na,CC>3/0.25 M NaHC03 buffer Std. # ' f t y f c - ' j - L . Dispense 5 ml of methyl-t-butyl ether TN-A- .w /L s --------------- Shake 20 min Shaker speed. -- _ Centrifuae 20-25 min. Centrifuge speed: 3CD^ Remove a 4 ml aliquat of organic layer Put on Nitroqen Evaporator to dryness I emperature. KQQm lemc. . Add methanol Volume 1 _ ^ _ TN-A- V ... Vortex 30 sec. . Filter usina a 3cc B-D syringe with a 0.2 urn filter into an autosampler vial -- \^ Cont. Cal. Verifications used same matnx as for std curve 1 1/ 10/12/99 Draft Attachment A ETS-8-4.1 Extraction of PFOS from Serum Form Completion , / BvVerified /[ { l . l r ll) l(l f t Sample Weights/ Volumes Prep Datela): 10/19/99 Analyst(s): SEE Sample Matrix: Rat Serum Method/Revision: ETS-8-4.1 Target Analyte(s): PFOS, PFOSA Sample ID 9R03230M ,Dv 1.Control 9R 03231M ,D yl,Control 9R 03232M ,D yl,Control 9R 03233M ,D yl, Control 9R 03234M ,D yl,Control 9 R 0 3 2 4 5 M ,D y 1,5m g/k g 9R 03246M ,D y 1,5 m g/kg 9R 03247M ,D y 1,5 m g/kg 9 R 0 3 2 4 8 M ,D y 1,5m g/k g 9 R 0 3 2 4 9 M ,D y 1,5m g/kg 9R03235M ,Dy4,Control 9R 03236M ,D y4,Control 9R03 23 7M ,D y4,Control 9R03238M ,Dy4,Control 9R03239M ,Dy4,Control 9R 03250M ,D y4,5m g/kg 9R0325 lM ,D y4,5m g/kg 9R 03252M ,D y4,5m g/kg 9R 03254-1M ,Dy4,5m g/kg 9R 03254-2M ,D y4,5m g/kg ....--------------------------- Study Number: TOX-145 Box: 99-206 Final Solvent &TN Number: MeOFl/TN-A-2945 Matrix Blank/Identiner: Rabbit Serum/99062-39 Rat Serum/99062-88 Inibal Voi. mL 1 G ry,<_ . _____ 1_______ ___________ Verified By: Comments M / f t ____________ < w # ____________________ 1 _ _______ _________________________ -- _______ _________________________ . ... l i_______ _________________________ \' \ ^ - r = r - = . ----------------------------- Summary of method: -- ^ sCP Notes: Review Date RtsI0199 FormCompletion Verified By Ion Pur Standard C urvo--FImhI PrrpDaieU): Aealvitfi): Semple M aini: Metbed/Reviaien: Target Analyte<i): Boi Munber: 10/ 1^ * SEE Rai Semiti ETS-8- i PFOS. PFOSA 99-206 Stedy .Member* TOX-145 C q n p o n i N einber: Final Salven! 4 TN Number: MeOH/TN-A-294S Blank Tumm/ldentifier: Rabbit Serum/99062-39 Rat Senim/99062-18 FC Mix Sid Appre. 0 500 ppm: FC Mi Sld A pprei. 5 00 ppm: FC Mi Sld A pprei. 50 0 ppm: Surrogate Sld A pprei. lOOppm: 0b06-l?-2 90016-17.1 99095.33 99086-13-11 A c u ii Concentrai o f Standard in th FC Mix PFOS PFOSA Std Conc PFOSEA Std Conc ug/mL ua/mL 0 5005 ug/mL 0 4997 0 5005 0 4997 5 005 4 997 5 005 4 997 $ 000 5 005 50 05 4 997 49 97 50 05 49 97 50 00 50 00 50 05 50 05 49 97 49 97 PFOSAA Std Conc ug/mL 0 4999 0 4999 4999 4 999 4999 49 99 49 99 49 99 49 99 EtFOSE-OH Std Conc ug/mL 0.5005 0 5005 5 005 S 005 5 005 50 05 50 05 50 05 $0.05 Blank a e n m initiai vaiarne (mL) for curves: Finiil autveut velam e (mL) far carves: I 00 100 M556 Std Conc ug/mL 0 5010 0 5010 5010 5010 5 010 50 10 SO 10 SO 10 50 10 All Am't Spiked mL 0 020 0005 0010 0020 0005 0010 0.015 0 020 nittal Vokun mL 1.025 1.010 1 015 1.025 1.010 LOIS 1.020 1 025 AU Fmai Vol. mL 1 00 I 00 1 00 I 00 I 00 I 00 1 00 1.00 1 00 PFOS 24 8 248 493 735 976 Lions o f Standards ia the sample marni PFOSA PFOSEA Std Cone Std Cooc. ng/mL ng/mL 4.93 4 9 2 9 77 9 75 24 8 24 7 49 2 97 7 97 5 248 247 493 492 736 735 977 975 PFOSAA Sld Conc ng/mL 493 9 75 247 49 3 97 5 247 493 735 975 EcFOSE-OB ' Std Cone ng/mL 4 93 977 24 1 49 3 97 7 241 493 736 977 MSS* Std Cooc. ng/mL 494 9 7 24.8 49 4 97 8 248 494 737 978 Sufregate Sld Cooc. ug/mL lot Safregate Final Cooc. ag/mL 496 AB Am t Spiked mL 0 005 Calculated Concentra inni o f Standards <n PFOS PFOSA Final Conc ng/mL ng/mL 501 100 100 25 0 2 5 0 50 1 250 500 750 1000 250 501 751 1001 | o mL fuul solvent volume PFOSEA PFOSAA Final Cooc. Final Conc. ng/mL ng/mL 5 00 50 0 100 10 0 25 0 2 5 0 500 500 100 100 250 250 500 500 750 750 999 1000 E ifO S E -O H Final Conc. ng/mL SOI 100 250 50.1 100 250 501 751 1001 MSS* Std Cooc. ng/mL SOI 100 25 l 50 1 100 251 501 752 1002 Surrogate Std Cooc ug/mL 101 Surrogate Final Cooc ng/mL 503 ----- AU A m t Spiked mL 0 005 ile used for MS/MSD Rat control *mua^9062-88 MS/MSD Cone, in the sample matrix PFOS PFOSA PFOSEA Final Conc. Final Cone Final Cooc ng/mL ng/mL ag/mL 248 ---------- 241---------- 247 248 248 247 pie used for MS/MSD' Rat control io u n A 9 0 6 2 > ll MS/MSD Cone, in the finsi solvent PFOS PFOSA PFOSEA Std Conc Std Conc Std Conc uem l ug/mL ug/mL 250 250 250 250 250 250 Initial Volume (mL): 1 00 PFOSAA EtFOSE-OB MSS* Final Conc Final Cooc. Std Cooc. ng/mL ng/mL ng/mL 247 248 248 247 248 248 Approx. Std Conc 50 0 ug/mL A m t Spiked Vol. (mL) 0005 Initial Volume (mL): 1 00 PFOSAA ElFOSE'OB MSS* Std Conc Sid Cooc Std Cooc ug/mL ug/mL ug/mL 250 250 251 250 250 251 Approx. Std Conc 50.0 ug/mL 1 dr V ietai A ft 4 r )t. Am t Spiked Vol (mL) 0 005 Final Vol. (m 1 00 Rts10199 ritti#(0ftIvFom Completion Verified DILUTIONS SUMMARY SHEET Study: TOX-145 Dilution Date/Analyst: MCH, 10/21/99 Box#: 99-206 ,, ' sam p le n u m b e r or descrpition 1:50 9R03245M , Day 1 ,5mg/kg D50 9 R 0 3 2 4 6 M , D a y 1, 5 m g / k g D 5 0 9 R 0 3 2 4 7 M . D a y 1. 5 m g / k g D 5 0 9 R 0 3 2 4 8 M , D a y 1, 5 m g / k g D 5 0 9 R 0 3 2 4 9 M , D a y 1, 5 m g / k g D 5 0 9R03250M , Day 4, 5mg/kg D50 9R 0325IM , Day 4, 5mg/kg D50 9R03252M , Day 4, 5mg/kg D50 9R 03254-IM , Day 4, 5mg/kg D50 9R03254-2M , Day 4, 5mg/kg D50 1: _ . . . _ _ - 1: . _ . _ _ _ . - 1: . _ . - Solvent/TN Number: M eOH, TN-A-2945 Extraction Date/Analyst: SEE, 10/19/99 Matrix/Timepoint: Rat Sera Days 1&4 1: _ - - D IL U T IO N S 1: 1: --------- -- C om m ents M //V Verified By A J/A rz in i _ J ______________________ i/ i __________________ t ldd-1 u -- ....-- ------------------------------------ --^ .... Z' \ L __________ ___________-- Notes: D50=20 uL sample + 980 uL MeOH. j j j ^ (o) Form Completion Verified Bv: < * it / o k j / f f i Extraction W orksheet ETS-8-6.0 Stnrlv # / /V -J Matrix A L i / L ' i . ' 7 Box# c? - 2 & WK/Dav A A DateSpiked/Analyst flA t //9 i i c -H20Blk - / -LiverBIk - I -6ppb-1 -12ppt>-1 I -30ppb-1 I -60ppb-1 -120ppb-1 -300ppb-1 I -600ppb-1 ' -900ppt>-1 / -1200ppb-1 S urrogate Std Approx ppm Actual/W ppm 5.0 ui 5 0 ul 5.0 ui 5.0 ui 5.0 ui 5.0 u! 5.0 ul 5.0 ul 5.0 ul 5.0 ui 5.0 ui FC Mix ! FC Mix FC Mix Comr nents Verified By aporox.0.5 ppm a p p ro x.5 ppm approx.50 ppm lactual ppm actual ppm actual ppm . in ^ 1 ! ^ 2 ul 1 4 ul 1 io ui 20 ul 1/ I (i.y/ iy # 9902A W -) ---------// i / / / / 1--------- -------- _____ l--------_____ !---------- f---------- -- 1i---------------- f"---------- / 40 ul L/ i y 7i 10 ul ----------/ j P ------- - 4 / ------------ i / I 20 ul y \ iy y 30 ul J .____________ 4 ul -- j \ --------------------- -I i \ I. J / ! ------- --------------------- j ; y> ~7------- j1------=--= " j i j -= = Liver Extraction Method ETS-8-6 0 Vortex 15 Sec. Pipette Matrix, spike with appropriate surrogate or FC-Mix Volume___ LlQL ml Pipette 1 ml of 0.5 M TBA, pH 10. pH= {/) Std Pipette 2 ml of 0.25 M Na?COV0.25 M NaHCO- buffeT Std #" Dispense 5 ml of methyl-t-butyl ether TN-A- Shake 20 min Shaker speed: Centrifuge 20-25 min. Centrifuge speed: f i/o /7 7?T Remove a 4 ml aliquat of organic layer Put on Nitrogen Evaporator to dryness Add methanol Volume i i 'O ml i emperature Room I emp~ TN-A- J-M r Vortex 30 sec. Filter using a 3cc B-D syringe with a 0 2 urn fitter into an autosam cier vial Cont. Cal. Verifications used same matrix as for stc curve D ate & Initials JZL 2 10/12/99 Draft Attachment A ETS-3- 0 E (traction of PFOS from Liver Form Completion Verified By S o u l o l a r / H Ion Pair Standard C u r v w -T iu u e i P rep Date!*): A n a ly a tls): Sam ple M u m : M eth o d/R ev ia io n : T arget Analyte!*): Do* Number: 10/25/90 , RWW Rabbit Liver ETS-8-6 0 See below 99-206 FC M ix Std A p prox. 0.500 ppm: FC M ix Std A p prox. 5 .00 ppm: FC M ix Std A p prox. 5 0.0 ppm: S u rrogate Std A pprox. 101 ppm: 99086-44-3 99086-44-2 99086-44-1 99086-13-11 Actual Concentrano* o f Standard* in the r C Mix PFOS PFOSA EtFOSE-OH Sid Cone Std Cone Std Cone ug/mL ug/mL ug/mL 0.5004 0.5000 0 5000 0 5004 0 5000 0 5000 0 5004 0 5000 0.5000 0 5004 05000 05000 0.5004 0 5000 0.5000 5.004 5.000 5.000 5.004 5.000 5.000 5.004 5.000 5.000 50 04 50 00 50 00 MS56 Std Cone u g/m L 0.5000 0.5000 0.5000 0 5000 0.5000 5 000 5.000 5.000 50.00 Calculated Concentration* o f Standard* in the sample matrix PFOS PFOSA E tF O SE -O H MS56 Std Cone. Std Cone. Std Cooc Std Cone. ng/g "g/g ng/g ng/g 6.14 6 13 6.13 6.13 12.3 12.3 12.3 12.3 30 7 30.7 3 0 7 30.7 6 1 4 61.3 61.3 61.3 123 123 123 123 307 307 307 307 614 613 613 613 921 1228 920 1227 920 122- 920 1227 Study N um ber: TO X I45 Equipm ent Number: Final Solvent A TN Number: M eOH/TN-A-2945 Rabbit L iver/99086-lJ-S M570 Std Cone. ug/mL 0.5000 0.5000 05000 0.5000 0.5000 5.000 5.000 5 000 50.00 M570 Std Cone. tji 6.13 12.3 30.7 61.3 123 307 613 920 1227 Blank liver initial density (g) for curve*: Final solvent volum e (m L) for curve*: M eFO SE -O H Std Cone. ug/mL 0.5000 0.5000 0.5000 0.5000 0.5000 5.000 5000 5.000 50.00 POAA Std Cone. u g/m L 0.5000 0.5000 0.5000 0.5000 0.5000 5.000 5.000 5.000 50 00 PFHS Std Cone. u g/m L 0.5000 0.5000 0.5000 0.5000 0.5000 5.000 5.000 5.000 50.00 0 163 1 000 All Am t Spiked mL 0 002 0.004 0 010 0.020 0 040 0.010 0.020 0.030 0 004 All Density g 0 .1 6 3 0.163 0.163 0.163 0.163 0 163 0.163 0.163 0.163 All Voi mL I 000 1.000 1000 l 000 1.000 1.000 1.000 1.000 1.000 M eFO SE -O H Std Cone. ng/g 6.13 12.3 30.7 61.3 123 307 613 920 1227 POAA Std Cone ng/g 6.13 12.3 30.7 61.3 123 307 613 920 1227 PFHS Std Cone. ng/g 6.13 12.3 307 61.3 123 307 613 920 1227 Surrogate Std Cone. ug/mL 101 Surrogate Final Cooc. B*/g 3098 All Am 't Spiked mL 0 005 Calculated Concentri on* o f Standards in the 1 0 mL final solvent volume PFOS PFOSA E tF O SE -O H MSS6 Final Cone. Final Cone Final Cooc. Final Cone. ng/raL n g/m L fig/ml ng/mL 1.00 1 00 1.00 1.00 2.00 2.00 2.00 2.00 5.00 5.00 5 00 5.00 10.0 10.0 10.0 10.0 2 0 0 2 0 0 20.0 20.0 50 0 50.0 50.0 50.0 100 100 too too 150 150 150 150 200 200 200 200 M570 Final Cone. ng/mL 1.00 200 5 00 10.0 20.0 50.0 100 150 200 M eFO SE -O H Std Cooc. ng/mL 1.00 2.00 5 00 10.0 200 50.0 100 150 200 POAA Std Cone. ng/ml 1.00 2.00 5.00 10.0 20.0 50.0 100 150 200 PFHS Std Cone n g/m L 1.00 2.00 5.00 10.0 200 500 100 150 200 Surrogate Std Cooc ug/mL 101 Surrogate l-inal Cone. ng/m l 505 All Am `t Spiked mL 0.005 Sample used for MS/MSD: M S/M SD calc. In matrix PFOS Final Cone. ng/g 300 300 N o MS/MSD Initial W t (g): 1.000 PFOSA EtFOSE-OH Final Cooc. Final Cone. ng/g ng/g 300 300 300 300 MS56 Final Cone ng/g 300 300 Sampie used for M S/MSD' M S/M SD calc. In solvent PFOS Final Cone. ng/R 50 50 No MS/MSD Inina! W t (g): 1.000 PFOSA EtFOSE-OH Final Cone. Final Cone. ng/g 50 ng/g 50 50 50 M5S6 Final Cone ng/g 50 50 Initial Volume (mL): 3.00 M570 M eFO SE -O H Final Cone Std Cone. n/g ng/g 300 300 300 300 6.00 POAA Std Cooc. ng/g 300 300 ImoxJ Volume (mL): 3.00 M570 M eFO SE -O H Final Cooc. Std Cone. ng/g 50 ng/g 50 50 50 POAA Std Cone ng/g 50 50 Approx. Std Cooc.: 5.00 ug/mL Ain't Spiked (mL) PFHS 0010 Std Cone ng/g 300 300 Density 0.167 Approx. Std Cone.: 5 00 ug/mL A m i Spiked (mL) PFHS 0010 Std Cone ng/g 50 50 n jln .1 Final Voi. 1.000 IP S E -l0 2 5 9 L iv -9 9 0 8 6 -4 4 -l.x ls I oi * r l n Extraction Worksheet ETS-8-4.1 Study # Matrix / b k , / Box# 9 9 - J r c WK/Day r ----------- C)ateSoiked/Analyst ? ? 9 -H20Blk - i -SeraBIk - / -5ppb - / -10ppb - / -2 5 p p b '/ -50ppb - / -100ppb- / -- -250ppb- 1 -500ppb - / -750ppb - / J / -1000ppb - / Surrogate Std Approx ppm Actual ppm 5.0 ui 5 0 ui FC Mix FC Mix FC Mix Comments Verified By approx.0.5 ppm approx.5 ppm approx.50 ppm actual ppm actual ppm actual ppm s ?4c/: -iz-3 ! /1/id 1 # 99e/c-V f-/ / /m U* t/ I / i a i| f\ tol a ____ A) A -------- \ -------- J. cn o c o c_ 5.0 ul 5.0 ul 5.0 ul 5.0 ui 5.0 ui 5.0 ul 5 0 u! 5.0 ul 1 20 ul 1 A3 A :' I ______ 1______L _ > ' _______ \ ______ 5ul_____ _______ \ ______ 1 10 ul _______ I _____ 20 u! k ____ r) 5 ul 10 ul 15 ul _______ 1 -- J -----------_ _ 1 ----------- / 20 ul /i \ -- -------------- --^ _ = 5= --- i / __ / ^ / ___ c__ / ^ -^ _______________ 1 i^ 1_ - i Serum Extraction Method ETS-8-4.1 Date & Initials Vortex 15 Sec. /o /ld 9 ~ 91 c" ' Pipette Matrix, spike with appropriate surrogate or FC-MIx Volume___x_g____ _m_l___ Pipette 1 mi of 0.5 M TBA, pH 10. p H = /^ Std. # Pipette 2 ml'of 0.25 M Na7C03/0.25 M NaHCQ3 PuffeT Std # 9 * 0 7 6 -, W Dispense 5 ml of methyl-t-butyl ether _______________ TN-A- J . 9 9 C Shake 20 min Shaxerspeed: Centrifuge 20-25 min. Centrifuge speed: ^ Remove a 4 ml aliquat of organic layer Put on Nitrogen Evaporator to dryness Add methanol Volume Temperature. f. ( TN-A- U zJL^T to lL i'l9 9 Vortex 30 sec. Filter using a 3cc B-D syringe with a 0 2 urn filter mto an autosamoier vTaT Cont. Cal. Verifications used same matrix as for std curve. 10/12/99 Draft Attachment A ETS-3-4 i Fx: action of PFOS 'rom Serum Form Completion Verified By iojif/W ion Pair Standard C urves-Fluidi Prep Date*): A naiyii(i): Sam ple Matrix: M ethod/Revision: T arget AnalytHi): Box Number: 10/25/99 rw w /? u, Rabbit Serum ETS-8-4 I Below 99-206 FC M ix Std A p prox. 0 .5 0 0 ppm: FC M ix Std A p prox. 5 00 ppm: FC M ix Std A p prox. 50 0 ppm: S u rrogate Std A p prox. 101 ppm: /c h 3 99086--U - 3 99086-14-2 9901604-1 99086-13-11 c? PFOS Std Cone 0 5000 0 5000 5 000 50.00 ng/mL 9 76 97.6 248 493 735 976 PFOSA Std Cone ug/mL 0 5000 0 5000 0 5000 5 000 5.000 5.000 50 00 50 00 50.00 50 00 E tF O SE O H Std Cone ug/mL 0.5000 0.5000 05000 5000 5000 5.000 50 00 50 00 50.00 50.00 M556 Std Cone. ug/mL 0.5000 0.5000 0.5000 5 000 5.000 5.000 50.00 50.00 50.00 30.0<r ion s o f Standards in PFOSA Std Cooc ng/mL VALUE' 4 93 9.76 97.6 248 493 735 976 ample matrix E tF O SE O H Std Cooc. n g/m L VALUE! 493 9.76 24 8 49 3 97.6 248 493 735 976 MS56 Std Cone. ng/mL VALUE! 4.93 9.76 24.8 493 97.6 248 493 735 976 Study Number: TOX I45 Equipment Number: Final Solvent A TN Number: M eOII/TN-A-2945 Blank T m u e/ldentifier: Rabbit Sera/TNA-1382 M570 Std Cone. ug/mL 05000 0.5000 0.5000 5 000 5.000 5.000 50 00 50.00 50 00 50.00 MeFOSEOH Std Cone ug/mL 0.5000 0.5000 0.5000 5.000 5.000 5.000 50.00 50 00 50.00 50.00 Blank serum initial volum e | b L) for curves: Final solvent volum e (m L) for curves: I 00 1.00 POAA Std Cone. ug/mL 05000 0.5000 0 5000 5 000 5.000 5.000 50.00 50 00 50.00 50.00 PFHS Std Cone ug/mL 0.5000 0.5000 0.5000 5.000 5.000 5.000 50.00 50.00 50.00 50.00 All Ain't Spiked mL 0.010 0.020 0 005 0.010 0.020 0.005 0.010 0015 0.020 Ail Initial Volume mL VALUfc! 1 015 1.025 1.010 1.015 1.025 I.0I0 1.015 1.020 1.025 All Final Voi. mL 1.000 I 000 1.000 1000 1 .0 0 0 1.000 1 .0 0 0 I 000 1.000 1.000 M570 Std Cone. og/mL VALUE! 4.93 9.76 24 8 49.3 97 6 248 493 735 976 MeFOSEOH Std Cone. ng/mL VALUE! 4.93 976 24.8 49.3 97.6 248 493 735 976 POAA Std Cooc. ng/mL VALUE! 4.93 976 248 493 976 248 493 735 976 PFHS Std Cone. ng/mL VALUE! 4.93 9.76 24.8 49.3 97.6 248 493 735 976 Surrogate Std Cone. u g/m L All Am t Spiked mL Surrogate Final Cone ng/mL 498 Calculated Concentrations o f 9 m i n PFOS PFOSA Final Cooc. ng/mL n g/m L VALUE! 5 00 5.00 10.0 100 25.0 100 250 500 750 1000 100 250 500 750 1000 the 1.0 mL final solvent volume EtFOSEOH MS56 Fumi Cooc. Final Cooc. B g /m l ng/mL VALUE! VALUE! 5.00 5.00 10.0 10.0 25.0 25.0 50.0 50.0 100 100 250 250 500 500 750 1000 750 1000 M570 Fuial Cooc. ng/mL VALUE! 5 00 100 250 50 0 100 250 500 750 1000 MeFOSEOH Std Cone. ng/mL VALUE! 5 00 to o 25.0 50.0 100 250 500 750 1000 POAA Std Cooc. og/mL VALUE! 500 10 0 25.0 500 too 250 500 750 1000 PFHS Std Cone. ng/mL VALUE! 5.00 to o 25.0 50 0 100 250 500 750 1000 Surrogate Std Cone. ug/m L 101 Surrogate Final Cone. ng/mL 505 All Ain't Spiked mL 0 005 pie used for MS/MSD: N o MS/MSD M S/M SD Cone, in the sample matrix PFOS PFOSA Final Cone. Final Cooc. ng/raL n g/m L 248 248 248 248 pie used for M S/M SD No MS/MSD M S/M SD Cone, in the final solvent PFOS PFOSA Std Cone. Std Cone ug/mL ug/mL 250 250 250 250 E tF O SE O H Final Cooc. ug/m l. 248 248 Initial Volume (mL): 1.00 MSS6 M570 MeFOSEOH Final Cone. Final Cone. Std Cooc. ng/mL ng/mL ng/mL 248 248 248 248 248 248 2.00 POAA Std Cone ng/mL 248 248 E tF O SE O H Std Cooc. u g/m L 250 250 Initial Volume (mL): 1 0 0 MS56 M570 MeFOSEOH Std Cone. Std Cone Std Cone. ug/mL ug/mL ug/mL 250 250 250 250 250 250 200 POAA Sid Cone. ug/mL 250 250 Approx. Std Cooc.: 50 ug/m l PFHS Std Cone. ng/mL 248 248 Approx. Std Cone . 50ug/m l PFHS Std Cone. ug/mL 250 250 J' Ain't Spiked Vot. (mL) 0 005 Am t Spiked Vol. (mL) 0.005 Final Vol. (mL) A IPSE-I0259Sct-99086-44-I xl io/ j r / t f I'rcp I)aic(s) A n ily ^ tli): - Sim ple M ain i: ~Juff b Method/Rcvision: Target Analyte!): f f r s /F * 4 Sample Extraction Sheet Study Number: Equipment Number: Notebook# and Page: Final Solvent: 7fJ-A-& lii Procedure Detail A 7>F***r /shi__ -JLa. p /~ 7u*f.a.ML. <^ * ---------------------------------------- ?oA*/r&>s - 7 ? < j g i , *J- T*** - r.to - y> ' -p p ^ ^ S -./T ` T*T7> -- f9oU -1 3 -tl ________________________________ T F * /T > o A A __________________________________________________ .... lo p p m . * - l a o o K S a t - U 1 ) - < - s ^7 f 4 ?" ________________________ p-/aoo X /x a e . PC ./o O " Z+Pp> S> ^ 7r Extraction-1 Template Review Date _________ EmporeExiraciionP3.xls Page I of Sample Extraction Sheet Prep l)ate(s Y . t f a f l j Analyxt(x): T * * Sample Matrix: <TfJ . tn Method/Revision: Target AnalvtelJ _____________ Pf>*___ Study Number: 7 Q K /y S ' Equipment Number: Notebook# and Page: Final Solvent: Procedure Detail *IU iU A Ifrsk f * . f `/ /< a j / + - < r - A c e /* * * Z `A T U - e z .* . t f o < M .i> -An-~ > Y < ts O A n4.J + o * aA *M+* JJ~y s YY \ . ____ f r X r i 4 f * * k -- i * ~ < 7r f a t r - / * 7?*> sr I ^ f S A . 4 ./a -fL * 6 r f Q * d y 5 t 'Z i t d - ^ <a 7,mL _ -fL iL . d 4 u \ v - * J ' t&CYt. Jo**. ' T U c z * . n u & c & J i m 7 > 'f L * TU. JlllJ-i J- sU* m J -------------------- ---------------------------------------------------------- ffc i* . 1 - T T a n - /* - c - f* /o o - m n -3^ -3 cJ 0 -T ^ -. - y 7 F * * /T tA * :T i s i * . f o g 6 *: /<> U K X g a . 6 ______= Z / l _________________________ 1)0*4. PlS ! " ---"------------------------------f-------/-M---6----x-----i-9--. /7a7d ^ ____ g : + _____________ S . - ______________________________________________ X v j r * ----------------------------------------------------- ' tMOppm- ^ l*a ^ 3 a s - c -t-lK i : - /o O ^ m ^ K O .O Z e '* U ~ iC U a o C. -- /o o * * L vr -- 'Z w * fcZ /v V 7^ Spile*. +** 'fa /fL E ^ *rcv< 9 *i U*4 kirfL Si^rv'oiiJc. fJOgj, - /3 - / / ___________ s J t^ u U*JL___ / S o * J - _____a r / A > P W k e / i I t ~ L J J t b * e d < + & -------- ____* / - c / - f t - ^ m j r a * ^ - .___ Xj U * . y C e ____________g - f y * 2 0Q Z Z. r . r tl 4 . . ^ * * -* - 3 * * & f a / l t U T C k* T h i < . IM a ,a C * r * e . c M U r fL . s . Q J o e 's f i '-[ % y < t T A g S jT iKC*rrcc-Hj - * K it - ____ / ^ V i//y Extraction' I Tempiale R ev ie w Dale_________ EmporeExtraciionP3.xls Page 1 of P r e p D a ta ! ): A n a ly 'IO ): S im p l M a trix : \lc fh o d /R a v i io n : T a r g e t A n alyt< > > : /0 = o jA J ir A A P r o c e d u r a O tta il Sample Extraction Sheet .S tu d y > u m b r- / 3 i > . / y s E q u ip m e n t N u m b e r: N o teb o o k * a n d P if< F in a l S o lv e n t: TaJ - a - f f ? / itL-lt 4 t.it.d tC <- / " / A e d o * * . 2 m/ a '7 L * a * ~ aCJa .S -------------------------- -ff' - f L r tJ - U ~ -aJ -, A oP d a .% >f A . ^ D : ! `i 2 i A ; o X K - f / * t / - g*s/*CS -JL,j t c J r t / I n r f f ------ 4 ^ 4 -- /<a-/rA K 7 r e it S ti~ 4 ZL - f o C .r j4 ~ ____ f A M /t tH i f - __________ d i/* J ls, c-<---------- ir r e t rtr^r - T ^S c -- 7 -F a S H er f? ? Z - / ~ / 4 4 fe C r / p e ^ - 7A o PPq s/F oaa. - ____________ . _____________________ 7 ^ t - / : ? O P / i ______ ____{ - Z f p b -------------- l l______________________ _____________________ / O l M - i f ______________________________ 0 - 5x> r ^ . * * > /' 'k u . w / J o o tttr U A { V. X /-_= --------- " -- ^ r tU > ( T f . rjJf^AA / 0 * - L- r ^ ..r . 'h e * - se 4 JHS jo Ff je 7- 2a*j _____________ ( t i n i . A fOOO -- .. 2ao 7^ f< * u ~ L 4 x f l - Q /P-m -Z . * J o o O ^ /Q O p o it Q fd s S jt /O fiA -L ------------------------------ Z____ ^ 3 x > to d * ** M i 4^ S O -+ A JK ,-p:/kA. UU XX --rrrrii <f =ra..r U- r er fJ____S L.r/L - M __Jnfo'J? --- / 3J ~ / tf .__/Potf l&tir-J.----------- ,r A&< ______ `nU bL Li rJ b. L. - ___ * 2 -- a . J ` 5&0 ^ i f / X > P P r*- 'S r / t tr / A - / 3 M r-Li - 4 * ^ ; t A - e Extraction! Template Review Oate______ E x tra c tio n xls / pj F o rm A p p ro v e d b y ^ a t ^ P i i { e I >('_________ Extraction Worksheet ETS-8-4.1 S|Mdy TOX 145 Matrix Rat Sera Rnx # 99-208 Surrogate Std FC Mix FC Mix FC Mix Comments Verified By Approx.100ppm approx.0.5 ppm approx.5 ppm approx.50 ppm Actuahci ppm actualc.~i ppm actual ^ c ppm actual sj c ppm DateSpiked/Analyst RBS11039-250ppb-CCV9&10 q q p fa -1 3 -n # ^ < < ^ - 4 7 -a W A A H/Oj I M 5 uL - -------- ---------- 47,U.'l/pi/^ - 5 uL & RTS11039-SeraBlk-9&10 RTS11039-250ppb-MS9 5 uL 5 uL - -- 5 uL RTS11039-250ppb-MSD10 5 uL - - 5 uL RBS11039-H2O8lk-9&10 5 uL - - - RBS11039-SeraBlk-9&10 RBS11039-5ppb-9&10 5 uL 5 uL 10 UL - - ---------- a______ RBS11039-10ppb-9&10 5 uL 20 uL - - RBS11039-25ppb-9&10 5 uL - 5 uL RBS11039-50ppb-9&10 5 uL - 10 uL - RBS11039-100ppb-9&10 5 uL - 20 uL RBS11039-250ppb-9&10 5 uL - - 5 uL RBS11039-500ppb-9&10 5 uL - - 10 uL RBS11039-750ppb-9&10 RBS11039-1000ppb-9&10 5 uL 5 uL - - 15 uL ____ ______ - 20 uL ____ _____ 4 / 9R03240M-0-Day 29 5 uL - - 9R03241M-0-Day 29 5 uL - - - ____ \ ------- 1 9R03242M-0-Day 29 5 uL - - - 9R03243M-0-Day 29 5 uL - - _____ __ &2m -- 9R03244M-0-Day 29 5 uL - - * _____ l -- L_9R03255M -5m g/kg-D ay 29 5 uL - - - ______ 9R03256M -5mg/kg-Day 29 _ 5 uL - -- - 9R03257M -5m g/kg-Day 29 5 uL - - - 9R03258M -5m g/kg-Day 29 5 uL - - - j- 9R03259M -5m g/kg-Day 29 5uL - - - *v Blank: Rabbit Sera Std# cW O ti R - 9 4 amount=t.O ml Serum Extraction Method ETS-8A1 : ________________________ Date & Initials-- Vortex 15 Sec. Pipette Matrix, spike with appropriate surrogate or FC-Mix Volume 1,0 ...ml IM-iA l ill'll iQAl-- Pipettel ml of 0.5 M TBA, dH 10. oH= ID ill ?/-?*? Std. `ROXLj - IH4i> Pipette 2 ml of 0.25 M Na,CO;j/0.25 M NaHC03 buffer Std. # Dispense 5 ml of methyl-t-butyl ether TN-A- Shake 20 min Shaker speed: 3QQ rpm - (K --------- -- rdlA Centrifuqe 20-25 min. Centnfuge speed: 35Qd rpm Remove a 4 ml aliquat of organic layer Put on Nitrogen Evaporator to dryness Add methanol Volume'-u! Temperature. R oom Tem p. ml TN-A-r-J'-'PlH i-- KJ 1A- Vortex 30 sec. Filter using a 3cc B-D syringe with a 0.2 urn filter into an autosampler vial Cont. Cal. Verifications used same matnx as for std curve. - J ______ V __ i L _____ FN-1: The MS/MSD and associated sera blanks were taken from control rat sera T C R ^ C v S , 'b C . vuu ii/c } /^ f m-J - v L i S u o i f N - ' `7 ' T <'ct\cc*r\ fter a nwoft TVa\ yxmpl-e. W*c\ not Lorvi^\et<r^ ctow m T p ^ f c i - c ' - r - i e r C\/"VV It - r\ ,s ^V\-c v^-<TV\ Ct 'S ^aa-vt- M | c i 1*1^ 10/12/99 Draft Attachment A ETS-8-4.1 Extraction of PFOS from Serum Form Completion Verified Bv / / / < / f ; I ion Pair Standard Curves-Serum P r rp D .ttU ) : 11/03/99 A n .lv , .): MCH Sam ple M .t m : Ral Sera M ethod/Reviaw n: ETS-8-1 I T arget Analyte<i): PFOS. PFOSA Box N u m b e r: 99*208 Srudy Num ber: TOX14S Equ.pm m it Num ber: F m ,i Solv' " ' & TN N u m b ,r: MeOH TN-A-2997 Bl* " k T iw ue/ldentifier: Rabbil Sera TCR99062-94 FC Mix Std A pprox. 0.500 ppm: 99086-47-2 FC Mix Std A pprox. 5.00 ppm: 99086-47-1 FC Mix Std A pprox. 50 0 ppm: 99095-33 S u rro g a te S td A p p ro x . 100 ppm: 9 9 0 86-13-11 Blank jen im initial volume (m L | for cu rv e,: Final solvent volume (m L) for curves: 1.00 100 Actual Concentrations o f Standards in the FC Mix PFOS PFOSA PFOSAA E tF O S E PFOSEA M556 All All All Std Cone. Std Cone. Std Cone. Std Cone. Std Cone. Std Cone. Am't Spiked Initial Volum Final Voi. ug/mL ug/mL ug/mL ug/mL ug/mL ug/mL mL mL mL 0.5000 0.5005 0.4997 0.4999 0.5005 0.5010 0.010 1.015 1.000 a 0.5000 0.5005 0 4997 04999 0.5005 0.5010 0.020 1.025 1.000 5.000 5.005 4.997 4.999 5.005 5.010 0.005 1.010 1.000 5.000 5.005 4.997 4 999 5.005 5.010 0 .0 1 0 1.015 1.000 5.000 5.005 4.997 4.999 5.005 5.010 0.020 1.025 1.000 50.00 50.05 49.97 49.99 50.05 50.10 0.005 1.010 1.000 50.00 50.05 49.97 _ 49.99 50.05 50.10 0.010 1.015 1.000 50.00 50.05 49.97 49.99 50.05 50.10 0.015 1.020 1000 50.00 50 05 49.97 49 99 50.05 50.10 0.020 1.025 1000 Calculated Concentrations o f Standards in the sample matrix PFOS PFOSA PFOSAA Std Cone. Std Cooc. Std Cone. ng/mL 4.93 ng/mL 4.93 ng/mL 4.92 9.76 9.77 9.75 24.8 24.8 24.7 49.3 49 J 49.2 97.6 97 : 97.5 248 248 247 493 493 492 735 736 735 976 977 975 E tF O S E Std Cone. g/mL 4.93 9.75 24.7 49.3 97.5 247 493 735 975 PFOSEA Std Cone. ng/mL 4.93 9.77 24.8 49.3 97 T ~ 248 493 736 977 M556 Std Cone. ng/mL 4.94 9.78 24.8 494 97.8 248 494 737 978 Surrogate Std Cone. ug/mL 101 S u rro g ate Final Cone. ng/mL 498 All Am t Spiked m l. 0.005 _ Calculated Concentrations o f Standards in the 1.0 m L final solvent volum e PFOS PFOSA PFOSAA E tF O S E Final Cooc. Final Cooc. Final Cone. Final Cone. ng/mL ng/mL ng/mL g/mL 5.00 5.01 5.00 5.00 10.0 10.0 10.0 10.0 25.0 25.0 25.0 25.0 50.0 50.1 50.0 50.0 100 t o o 100 1 0 0 250 250 250 250 500 501 500 500 750 751 750 750 1000 1001 999 1000 PFOSEA Final Cone. og/mL 5.01 10.0 25.0 50.1 100 250 501 751 1001 M556 Std Cone. og/tnL 5.01 10.0 25.1 50.1 100 251 501 752 1002 S u rro g ate Std Cone. ug/mL 101 Surrogate Final Cone. ng/mL 505 All Am't Spiked m l. 0.005 Sample used for MS/MSD: TCR99062-30 MS/MSD Cone, in the sample m atnx PFOS PFOSA Final Cone. Final Cooc. ng/mL ng/mL 248 248 248 248 Sample used for MS/MSD: TCR99062-30 M S/M SD Cone, in the final solvent PFOS PFOSA Std Cone. Std Cooc. ug/mL uaraL 250 250 250 250 PFOSAA Final Cone. ng/mL 247 247 Initial Volume (mL): 1.00 E tF O S E PFOSEA MS56 Final Cone. Final Cone. Std Cone. ng/mL ng/mL ng/mL 247 248 248 247 248 248 Approx. Std Cooc.: 50.0 ug/mL Ain't Spiked Vol. (mL) ___________________ Initial Volume (mL): 1.00___________ PFOSAA E tF O S E PFOSEA M556 Std Cone Std Cone. Std Cone. Std Cone. ug/mL ug/mL ug/mL ug/mL 250 250 250 251 250 250 250 251 Approx. Std Cone : 50.0 ug/mL Am t Spiked Vol. (mL) 0.005 Final Vol. (mL) I 00 Toxl45 U,: - ^ DILUTIONS SUMMARY SHEET Study: TOX145 Dilution Date/Analyst: 11/5/99 M C H M * ^ " P I B o x tt: 9 9 - 2 0 8 S o l v e n t / T N N u m b e r : M e O H T N - A - 3 :Y&Ip Extraction Date/Analyst: M C H 11/3/99 M atrix/Timepoint: Rat Sera Day 29 Notes: D10=100 uL sample + 900 uL MeOH. flW *l{SJ*!0! Form Compjgtion . V e r ifie d B y I\ A ' * - ` !- /*h A mV ' ' Extraction Worksheet ETS-8-6.0 //// Sturiv# TOX-145 Surrogate Std Matrix Rat Liver___________ Approx, ppm Box# 99-211 Actual/# / ppm FC Mix FC Mix FC Mix approx.0.5 ppm approx.5 ppm approx.50 ppm actual ppm actual ppm actual ppm Comments Verified By WK/Dav Dav 29 # W /> U i3 J l # 7 9 & C -W .J # ? ? (/< , / y - z # /// DateSpiked/Analyst fh u /M 9 - -C C V -/W -2 $ / ! / } ./ J '/C -MS- -MSD-H20Blk-1&2 -LiverBlk-1&2 -6 ppb-1& 2 - 1 2 ppb-1&2 h/j A + - X w 5.0 ul 5.0 ul 5.0 ul 5.0 ul 5.0 ul 5.0 ul 5.0 ul 1/ / /O k , - m J 10 ul 10 ul 10 ul 7! z ___________ _________ / _ ' 2 ul / 4 ul / . I . . . ..... CiL ___ ___ J -------------- /V / liLlA- M l / M z _______ / / -30ppb-1&2 -60ppb-1&2 -12 0 ppb-1&2 -300ppb-1&2 5.0 ul 5.0 ul 5.0 ul 5.0 ul 10 Ul 20 ul 40 ul ^ / / _____ / __________ ____ i z p ____ 10 ul / -600ppb-1&2 5.0 ul AO 20 ul / -900ppb-1&2 z - 1200ppb-1&2 5.0 ul . 5.0 ul / / 30 ul / 4 ul A A^ Sample numbers and weights noted on a separate page - add S'0 ul surrogate to ail samples. / /4---------- --j -- --- -- */'// y r / v ^ --------- Blank - O j /, , } - / < s td # ? ? z T ^ 7 7 -. Liver Extraction Method ETS-8-6.0 amount = A r) ml ), / 3 g/ml Date 81 Initials Vortex 15 Sec. Pipette Matrix, spike with appropriate surrogate or FC-Mix Pipette 1 ml of 0.5 M TBA, pH 10. pH= Pipette 2 ml of 0.25 M Na?CQr,/0.25 M NaHCO-, buffeT Volume / T o ' ml s td . n _2S e2A .i l Std. V9L V 4 5 T i h ? ~ / -cJ aA A ///// 9 Dispense 5 ml of methyl-t-butyl ether TN-A- 9 V C Shake 20 min Shaker speed: 1 / ) D Centrifuge 20-25 min. Centrifuge speed: i T o D Remove a 4 ml aliquat of organic layer Put on Nitrogen Evaporator to dryness Temperature: Room Temo. Add methanol Volume ! ,r? ml TN-A- J - f ? 7 Vortex 30 sec. Filter using a 3cc B-D synnge with a 0.2 um filter into an autosampler vial Cont. Cal. Verifications used same matrix as for std curve. UN w U j .u Illesi ^ W UJL EEpS' \T~ 10/12/99 Draft Attachment A ETS-8-6 0 Extraction of PFOS from Liver Form Completion . Verified Bv h U A t ( Q'-l t\ Sample Weights/ Volumes s* ! + > r\ i / -- i / Z y / r f - / v - v PrepDate(s): 11/3/99 Analyst(s): RWW Sample Matrix: Rat Liver Method/Revision: ETS-8-6.0 Target Analyte(s): PFOS, PFOSA Sample ID 9R03240/M/Day29/Control 9R03241/M/Dav29/Control 9R03242/M/Day29/Control 9R03243/M/Day29/Control 9R03244/M/Day29/Control 9R03255/M/Day29/5mg/kg 9R03256/M/Day29/5mg/kg 9R03257/M/Day29/5mg/kg 9R03258/M/Day29/Smg/kg 9R03259/M/Day29/5mg/kg _______ ______________ Initial WL g (, OXo 2 /, W 7 ///? $ ' / 1JYu/ /. iZ fO /, /JL O ? Z >Y /? . MO Water ml 5 ml 5 mi 5 ml 5 ml 5 ml 5 ml 5 ml 5 ml 5 ml 5 ml Study Number: TOXI45 Equipment Number: Final Solvent & TN Number: MQ Water Matrix Blank/Identifier: Rabbit Liver/99086-13-5 Box: 99-211 Verified By: Comments ------------------ - -- ^ -- ___________ / HP1 / S' -- ----------------------------- ) J T /W ^ ___- -- ------------------------- ---------------------Summary of method: Notes: Review Date Form Approved by/Date: Weight Volume Sheet-101299.xls Form Completionn Verified By // 11 i 111 ion Pair Standard Curvev-Ttssucs 0 S K / , , / - /////< ? f Prep Dateti): Anaiyit(i): Sampie Matrix: Mefhad/Rcvtsion: Tarpet Aoaiyte(i): Bos Number: 11/4/99 RWW /<tx.' *\/ Rabbit Liver ETS-8-6 0 See below 99-211 a f'/U ? FC M il Std Approx. 0 500 ppm: FC Mix Std Approx. 5.00 ppm: FC Mix Std Approx. 50.0 ppm: Surrogate Std A pprox. 101 ppm: 99086-44-3 990S6-44-2 99016-U-l 9908^13-11 Actual Concentrations o f Standards in the FC Mix PFOS PFOSA EtFOSE-OH Std Cone Std Cooc Std Cooc. ug/mL ug/mL ug/mL 0.5004 05000 05000 0.5004 0 5000 05000 0.5004 0.5000 05000 0.5004 0.5000 0.5000 0.5004 0.5000 0.5000 5.004 5.000 5 000 5004 5.000 5.000 5.004 5.000 5000 50 04 50.00 50.00 M5S6 Std Cone. ug/mL 0.5000 0 5000 0.5000 0.5000 0.5000 5000 5.000 5.000 50.00 Calculated Concentra Dons o f Standards ui the sample matrix PFOS PFOSA EtFOSE-OH M5S6 Std Cone Std Cone. Std Cooc. Std Cone "/g ng/g ng/g g/g 6.14 6.13 6.13 6.13 12.3 12.3 12.3 12.3 30.7 30.7 30.7 30.7 614 61.3 61.3 61.3 123 123 123 123 307 307 307 307 614 613 613 613 921 920 920 920 1228 1227 1227 1227 Study Number: TOXI4S equipm ent Number: Final Solvent Sl TN N um ber: MeOH/TN-A-2997 R abbit Liver/990B6-13-5 MS70 Std Cone. ug/mL 0.5000 0.5000 0.5000 0.5000 05000 5.000 5.000 5.000 50.00 M570 Std Cone. ng/g 6.13 12.3 30.7 61.3 123 307 613 920 1227 Blank liver initial d o luity (g) for curves: Final solvent voluac (m L) for curves: M eFO SE -O H Std Cone. ug/mL 0.5000 0.5000 0.5000 0.5000 0.5000 5.000 5.000 5.000 50.00 po a a Sid Cooc. ug/mL 0.5000 0.5000 0 5000 0.5000 0.5000 5.000 5.000 5.000 50.00 PFHS Std Cone. ug/mL 0.5000 0.5000 05000 0.5000 0.5000 5.000 5.000 5.000 50.00 0 163 1.000 All Am't Spiked mL 0.002 0 004 0.010 0.020 0040 0010 0020 0.030 0.004 At; Density 8 0.163 0.163 0.163 0.163 0.163 0.163 0 163 0.163 0.163 A ll Vot. mL l I l. I. I. 1. 1 I. M eFO SE -O H Std Cone. ng/g 6.13 12.3 30.7 61.3 123 307 613 920 1227 POAA Std Cone. ng/g 6.13 12.3 30.7 61.3 123 307 613 920 1227 PFHS Std Cone. ng/g 6.13 12.3 30.7 61.3 123 307 613 920 1227 Surrogate Std Cone. ug/mL 101 Surrogate Final Cone. "g/g 3098 All Am't Spiked mL 0.005 Calculated Concentrations o f Standards in the 1.0 mL final solvent volume PFOS PFOSA EtFOSE-OH M556 Final Cooc. ng/mL Final Cone. ng/mL Final Cone. wg/ml Final Cooc. ng/mL 1.00 1.00 1.00 1.00 2.00 2.00 2.00 2.00 5.00 5.00 5.00 5.00 10.0 100 100 10.0 20.0 20.0 2 0 0 20.0 500 50.0 5 0 0 5 0 0 100 100 100 100 150 150 150 150 200 200 200 200 M570 Final Cooc. ng/mL 1.00 2.00 5.00 10.0 20.0 50.0 100 150 200 M eFO SE -O H Std Cooc. itg/ml 1.00 2.00 5.00 10.0 20.0 50.0 100 150 200 POAA Std Cooc. wg/tnl 1.00 2.00 5.00 10.0 20.0 50.0 100 150 200 PFHS Std Cone wg/ml. 1.00 2.00 500 10.0 20.0 500 100 150 200 Surrogate Std Cone. ug/mL 101 Surrogate Final Cone. wg/ml. 505 All Am't Spiked m l. 0.005 Sample used for MS/MSD: 9R03240 MS/MSD calc. In matrix_____ Initial W t (g): 1.020________________________ Initial Volume {mL): 5.00 PFOS PFOSA EtFOSE-OH M556 M570 M eFO SE -O H Final Cooc. Final Cooc. Final Cone. Final Cooc. Final Cone Std Cooc. ng/g ng/g ng/g ng/g "g/g ng/g 295 295 295 295 295 295 295 295 295 295 295 295 6 00 POAA Std Cone. ng/g 295 295 Sample used for MS/MSD: MS/MSD calc. In solvent PFOS Final Cone. ' ng/g 500 50.0 9R03240 Initial W t (g): 1.020 PFOSA EtFOSE-OH Final Cone. Final Cooc. "g/g g/g 500 500 500 500 MSS6 Final Cone. ng/g 50.0 50 0 Initial Voiiane (mL): 5.00 MS70 M eFO SE -O H Final Cone Std Cone. ng/g ng/g 500 500 500 500 6.00 POAA Std Cone. ng/g 500 500 Approx. Std Cone : 5.00 ug/mL Ain't Spiked (mL) PFHS Std Cone. ng/g 295 295 Density Approx. Std Cone.: 5.00 ug/mL Ain't Spiked (mL) PFHS Std Cone. ng/g 50.0 50.0 Final Vol. IPSE-10259Liv-99086*44-1 xls DILUTIONS SUMMARY SHEET Study: TOX-145 Dilution Date/Analyst: SAL 11/9/99 Box#: 99-211 Solvent/TN Num ber: MeOH TN-AExtraction D ate/A nalyst: RW W 11/4/99 M a trix /T im ep o in t: Rat Liver Day 29, Grp 6 FACT: DATA REVIEW SUMiMARY FORM ^ ^ r U z Date: Data Analyst: Data Review Sign-Off *Analyst Review Name / Date: FACT Study#: Matrix/Timcpoints: 2 / S r y c -~'Bm Sample List: h /9 i? k SeMip Analysis Date/Analyst i /n /i9 M nU instrument ^ J tlv Analvte: 7oAA ( C H l'f Acceptable Linear Ranae: Ad *" s* 0* 0L-fs LOO: A/A Extraction Blank: kJA RA2: A/A Matrix Blank: AX Calibration Checks: A/fl MS/MSD: (g l ">\AK Data Status: rn S LL r>DMiihra>W. ^ lo jiilw Analyte: TfbS (Hz') Technical Review Name / Date: ff)33E Quality Assurance Review Name/ Date:_________ Data Entry:. 1A L _____ 1 0 u l f t Comments/ Justifications: 0 /I CtlriH lots A./~ ru* i/e/- fla. OmJ ucIs tri ~p0AA. /Lu. d a ft, /S Ok-L T f a r lo a k iK j a / -3a - g y r e . ffa tu M ' 3 * e ,0 /r * /r > . Tl i s va h ^ 0 ,n J - k /tS d ra a p et/_______ ie e a n s t / / A/cr 0 Js,</c, -U * tin ta r ya.r a t __ / ,, q J - 'L L C u ru e . ` " V f ___f l i e r u o i X r C f S ___ jr * b a (e 3 i * > / /W < ? / . K t / t e e t / / a . - f i t O a & tJ S a-t*-7>les ju L / - ________ 4* PU att i/a r d c s f //f J /r j__t4 d s S a c f_____ Acceptable Linear Range: l L f f k WeL LOO: i Jjpr.1 Extracted Blank: Ifss -/a *- 3$ R - 2 : t i n s s e _________ Matrix Blank: rs -La *. Loci S cia it U s f a .* - j d - 4 L S ~ j> r e * - d l/Ujlt arra L'oh.rJs d u s/ ustrt OuJ-eiJe 4/u fUa*tJ'i-hdiax-. 3-S '`/r-Zri Calibration Checks: fi S y ,* f "'*" *~/ _____ ^ 7L 73 >i >La*.J p**-i4 ______ MS/MSD: Data Status: H L D lk W r ntirllA M ><r 'U t ....& t * r g s c e a u * * - _________ t W rvimftls ^ 1 J L Uir** ouJ-SiJc 4L //usar yg_HJS.___ W Analyte: TpoSA. CfU-') Acceptable Linear Range: LOQ: j ? 3 P>L R -2: Q m t 7 9 Calibration Checks: f)K - MS/MSD: Data Situs: L ~!ka M i H b /* * -L s l x e .J -fiD r/u /t /jL_ Extracted Blank: fla t. o<3 Matrix Blank: /ess '//g a . LoQ -/3 % > /" / , LAC ip ,' ^ h Ai / * / s J 7 f s a . ~ T * ' z * /? * ___________ PoA A axauX A * a ^ c / u y J c x K f ' . Q \iO M \u M (M i n n L ld L r d j t^ C U l m C h (fC (& <fr.\ matri f o r u f w A i c t f < g t o C u i _____ ^ ^AA. I Ql T j f _________ FACT: DATA REVIEW SUMMARY FORM Date: i^ lz - h Dala Analyst: FACT Study#: Matnx/Timepomts: - L /fV -C * * U k< {~ - - e * t. % h l Sample List: h r tllL __________________________________________ ____ Set-up Analysis Date/Analyst: Instrument , A v ? / M*iW_____________________ ?Y->y, 02>/?? Analyte: CcH</ _____________________________ Acceptable Linear Range: fJA____________________________ LOQ:_________a <A Extraction Blank: Ata RA2 :_________ /A__________ Matrix Blank: stA Calibration Checks: ______ A/A____________________________ MS/MSD:___________________ ~~-------------------------------------- Data Status:__________ *^ Data Review Sign-Off Analyst Review Name/ Date: _____ Technical Review Name/ Date:___ S /A J lf ly , l ftP 1 LAC lo lv h Quality Aararance Review Name/ Date:_________ DataEntry: IAC lo/zilW . Comments/Justifications: __________________ s U a tfA - l a c k ___________ dAci-lfK./ . A f f S ~ y > lt5 . Carves f C*J fifu e ju it* * / /n u d /tu * p i 3*> A o r / e s i . '" J a s lo/ J n _____________________________ > M- 232S23S?333 S32?"2 S22SS7 S2S|2? ;o32K SKT 527 "777" 7" VSS S S S S 3S P S S S 3S 3 3 S g g 3 -3 3 3 SSSoSo SSSSSS 2 r 7 2 7 7 7 7 <r 4 r4 O O < '" ' - --- *"* n n aaaaaaaaaaaaa aaaaaa aaaaaa aaaaaa aaaaaa aaa aaaaaaaaaaaaa ;S3S5323SSS3S 222332 S5222S SSSSS3 22322" 23" S2S33S3333SS3 1 3a3iasS33aa3 l a a i a i s a sa ss as ia as s i i s a a aaa aaaiaaaaaaasa 3 - r - - .-r-r- r. S ggggSSSSS o o o 7 ^^3333 <3 O 3 \\ - %* M SEBES ;lticli; ss 33333 77777 ESEES mt?i??l5 33333 77777 ggg bBS "222 ?S333b saSEE 5 52223 ES I? 22 S3 S2332a ^ ,3 3, ,,3 3 .l , , , , ,, % l i l i l S i l m B 3 j | 5 , m h * ilil^mll sss*| 58iKj!1KSSiK! asi l-irtiJl i i i m 1ISI IfiSil lili? M illffii! 1 SSBSSSSE lisc HIISS jjlH S 81ISSS ss =p=s3ss:ss iiiiiiiiir m m m i i ..................... 02019t: Qoaat.a *nd pr;it' cowprwiwlO v M t l f y n-- n r *poit T O U I S - r K rt, dy 1 * 4 , cor.^ro'. . JR.. 10/19/99 I l a ^ l a List: C:\MASSLTXX\sout*rats.proNi >lsDB\101b |*St aodiflsd: Mad Oct 20 07:37:33 1999 netted: C: \HkB81TKt\sour -r*t % .pro\MathDB\101999b L u t wdifiad: *4 Oct 20 07:3i:46 1999 Job Coda: Frlntsd: . Oct 20 08:0:10 1999 101999012 101999013 101999014 101999026 16 101999027 17 101999028 19 101999030 20 101999031 21 101999032 22 101999033 23 101999034 24 101999035 2S 101999036 26 101999037 27 101999038 28 101999039 101999040 30 101999041 31 101999042 32 101999043 33 101999044 34 101999045 35 101999046 36 101999047 37 101999048 38 101999049 39 101999050 40 101999051 42 101999053 43 101999054 44 101999055 45 101999056 46 101999057 47 101999058 46 101999059 49 101999060 50 101999061 51 101999062 52 101999063 53 101999064 54 101999065 55 101999066 56 101999067 57 101999068 5a 101999069 59 101999070 60 101999071 61 101999072 62 101999073 MeCK Blank MeCK Blank MeCK Blank TC>:l45-RBS101r 9-h :; Blank-ll, SIE TC-US-RBSIO:'1 1-Se r a Blank-ll. SES TC.IHS-RTSIOI Cira Blank-ll. SES TCK145-RTS101r )-Sera Blank-12, SEE TCX145-RBS131' >-S.co-ll. SEE Tc:.:45-RBSicr -:.',pb-ll, SEE t c :-:;45-r b s i o :> *::jpb-11. SEE TC ::115-RBS101" -;.tpb-11, SEE TOX145-RBS1019 J-lOOppb-ll. SEE TOX145-RBS101f 9-250ppb-ll, SEE TOX145-RBS101'''-ECCppb-ll. S U TOX145-RBS1019 ?-750ppb-ll, S U TOX145-RAS101*)-1030ppb-ll, S U MeCH Blank TOX145-RTS, 9R03233M. Dyl, Control,-10/19/99 S U TCX145-RTS, 9? 33231M, Dyl. Control. -10/19/99 S U TCX145-RTS, 9R 33232M. Dyl, Control, -10/19/99 E U TOX14S-RTS, 9R03233M, Dyl, Control, -10/19/99 S U TCM145-RTS. 9R03234M, Dyl, Control,-10/19/99 S U Tc:-;145-RBS1019 3-20ppb-CCV-ll-l, S U MeCH Blank TC.115-RTS. 57 C323 SM, Dy4. Control,-10/19/99 S U TC..115-RTS. 9C 3323M, Dyi, Control, -10/19/99 S U TC 14S-RTS, SC Dy4. Control,-10/19/99 S U TC.:il5-RTS, 5' 3?:7M, Dy4, Control,-10/19/99 S U Tc:::is-RTS, 9- :3::;-m . Dy4, Control.-IO/19/99 S U t c ::i 15-RBSio: -C i ppb-CCV-ll-2, SES Me:H Blank TC 145-RTS 101' -CI.ppb-KS-ll. 10/19/99 S U TC:' 145-RTS101' -:::ppb-MSD-n. 10/19/99 s u TC':115-RTS. 5 3:;5M, Dyl, 5 ag/kg 10/19/99 S U Tc::i45-RTS, 9: :3:.?M. Dyl, 5 ag/kg 10/19/99 S U TC 145-RTS, 9r.332H H , Dyl. 5 ag/kg 10/19/99 S U TC :115-RBS101' 1 5: ppb-ccv-n-3, s u M<_:h Blank TC 115-RTS, 9? Dyl, S ag/kg 10/19/99 S U TC 115-RTS. S- Dyl. 5 mg/kg 10/19/99 SEE Typa Standard Standard Standard Standard Standard Standard Standard Standard Standard OC oc oc TC 115-RTS. 5* :3:::m . Dyi. 5 ag/kg 10/19/99 S U T 115-RTS. 51 :3:c :m . Dy4. 5 ag/kg 10/19/99 S U T .15-RBS10: '-l::ppb-CCV-ll-4. SEE H. Blank is -r t s . Zii-lH. Dy4. 5 ag/kg 10/19/99 SEE TC .15-RTS. - C:::-2M. Dy4. 5 ag/kg 10/19/99 S U r h s -r s s i c i :ppb-ccv-n-i. s u M . : Blank TC :i5-RBS10: - M J Blank-ll, SEE t c ..:;5-R3s i c :' Blank-ll. SEE t : 15-r t s i c : ra Blank-ll. SEE t c :;s -r t s i o : .a Blank-12. SES t : ::i5-R3Si:. ;b-ll. SES TC .15-RBSlC: -1 Tpb-ll. SSE T" .15-R3S1C1 -;=jpb-ii. s e e T" 15-RBS 10 1. -5:ppb-ii, s u TC...15-R3S1C1' -:.:ppb-n. s e s T . 15-RBS101 r -Crlppb-U, SSE T. 115-RBSlO: ':;ppb-ll, SEE TC. -.15-RBS10: -'T.ppb-ll. S U TO: 15-RBS101 -1 :)0ppb-ll. SEE oc oc Standard Standard Sraiwlard Standard Standard Standard Standard Standard Standard td Case 4.93 9.77 24.80 49.30 97.70 248.00 493.00 736.00 977.00 248.00 248.00 248.00 248.00 248.00 4.93 9.77 24.80 49.30 97.70 248.00 493.00 736.00 977.00 RT 7.836 7.806 7.853 7.833 7.839 7.822 7.834 7.808 7.813 7.810 7.802 7.814 7.811 7.809 7.814 7.813 7.877 7.836 7.834 7.808 7.832 7.837 7.812 7.854 7.856 7.837 7.8S2 7.8S8 7.852 7.806 7.854 7.789 7.803 7.791 7.790 7.814 7.809 7.881 7.80S 7.791 7.804 7.789 7.814 7.856 7.813 7.792 7.811 7.857 7.854 7.851 7.833 7.859 7.814 7.813 7,811 7.813 7.805 7.613 7.791 7.786 7.811 k m Flags 2725 Ml Cone. 2.28 1.04 U .Jfe 2036 MM 5196 MM 9S1S MM 16241 MM 100839 MM 117401 ioa 149225 KMX 226 Ml 142 Ml 49041 MM 312 Ml 168 Ml 139 MM 167 MM 146 MM 136 Ml 43165 Ml 315 MM 48811 MM 52881 MM 52155 Ml 87504 MM 51116 dd 49904 MM 384 MM 67032 db 55570 MM 11759 dd 15158 Ml 46625 MM 307 MM 12235 bd 11895 MM 50283 MM 348 MM 145 MM 126 MM 120 MM 148 MM 1139 MM 2063 NN 5615 MM 10041 MM 18028 MM 51069 MM 100103 Ml 122134 MMX 153334 MCX 9.76 -0 3 -4 585.80 -20 744.71 -24 0.30 0.32 0.27 215.13 1.17 243.32 -13 260.01 436.52 254.83 248.78 1.S1 334.30 277.07 0 58.31 75.28 232.41 1.13 60.69 58.99 250.67 1.33 0.32 0.23 0.19 0.34 5.26 9.90 27.63 49.73 89.61 254.60 499.43 609.44 765.23 -6 1 7 1 11 1 -8 3 1 -17 -22 Boup 020199: Quantified Od pr by l u on 10/19/99 A u jiitify CevOttB *pc : - , . . ... . TOEO*5-r*t aara, day I * 4, ccr.irol * do- t - 10/lt/M l ,1# C:\IOIStTMX\lov:-r*..proNa^lOU01ffb . . w^i.ld* wad O n 20 07:^":33 1 I M >>tthn|1. c: \HRSSt.TIX\ou; -rat* .pro\M*tdOM0H#*b t_..r edified: Wd OCt 20 07 :3: :4* 1** Job Coda: printad: 1 OC*. 20 08 :C ::10 1999 4: IS <Cb4) 1 101999012 2 101999013 1 101999014 4 101999015 5 101999016 6 101999017 7 101999018 8 101999019 9 101999020 10 101999021 11 101999022 12 101999023 13 101999024 14 101999025 15 101999026 16 101999027 17 101999028 18 101999029 19 101999030 20 101999031 21 101999032 22 101999033 23 101999034 24 101999035 25 101999036 26 101999037 27 101999038 28 101999039 29 101999040 10 101999041 31 101999042 32 101999043 33 101999044 34 101999045 35 101999046 36 101999047 37 101999048 38 101999049 39 101999050 40 101999051 41 101999052 42 101999053 43 101999054 44 101999055 45 101999056 46 101999057 47 101999058 48 101999059 49 101999060 50 101999061 51 101999062 52 101999063 53 101999064 54 101999065 55 101999066 56 101999067 57 101999068 58 101999069 59 101999070 60 101999071 61 101999072 62 101999073 S W l a l i s t T-' MaOH Blank MaOH Blank MOII Blank TOX14S-RBS10'- ?-HlD Blank-ll. SEE TOX14 5-RBS i-Sera Blank-ll, SEE TOX243-RTS1:: -S-:s Blank-ll. SEE TOX145-RTS1:: -Sera Blank-12, SEE TOXl-i^-RHSlOl --pb-11. SEE TOXI;5 -R93 i: . '-llrpb-ll. SEE TOXll ;-RESlt1' l-lrpb-ll. SEE TOXi;-RBs::: }-5:?pb-ll. SEE TOXli 5-RBSKI )-110ppb-ll. SEE t o x i ;s -r b s i c : >-:!3ppb-il. SEE TOXliS-RBSlC: '-S !Oppb-11. SEE TOXI-5-RBS101 -75Jppb-11. SEE TOX1.5-RBS101 3-i:30ppb-ll. SEE HeOB Blank TOX145-RTS, 5: 33250. Dyl. Control.-10/19/99 SSE TOX145-RTS, 9 33221, Dyl, Control.-10/19/99 SSE 10X14 5-RTS. 9!.33222. Dyl. Control,-10/19/99 SEE TOX145-RTS, 5: 33233, Dyl. Control.-10/19/99 SSE TOX145-RTS. 5. 332;4M, Dyl, Control.-10/19/99 SES TOXli:-RBS101 .'-22ppb-CCV-ll-l, SIE HaOH 3lank TOX141-RT3. c Dy4, Control.-10/19/99 SEE TOXI 5-RTS , .3216, Dy4. Control.-10/19/99 SEE TOXI -RTS . ill'M. Dy4, Control.-10/19/99 SEE t o x i ;.-"3. Dy4, Control.-10/19/99 SEE TOXi;'-RT2, ` 32 -M, Dy4, Control,-10/19/99 SEE t o x i ;!-r s s ::i -21 .'ppb-CCV-11-2, SEE MaOH 31ar.t t o x i ;5-r t s ::: '-2:2ppb-S-ll, 10/19/99 St* t o x h b -r t s i :: -2:3ppb-SD-11. 10/19/99 SEE 5. Dyl, 5 wg/kg 10/19/99 SEI Dyl. 5 wg/kg 10/19/99 t o x i ;>--RB3101.'-253ppb-CCV-ll-3. SEE HaOH 3!lan'< -RTS, : '32;EM, Dyl. 5 wg/kg 10/19/99 -RT3. 32;?. Dyl, 5 ng/kg 10/19/99 -RTS. - Dy4, 5 ag/kg 10/19/99 RTS. '`IM. Dy4. 5 wg/kg 10/19/99 t o x i ; ..3--' < 231 -2M. Dy4, 5 wg/kg 10/19/99 TOXI;:-R52i:- :;.;ppb-ccv-n-4. s e e McOH -R75. Dy4 . 5 mg/kg 10/19/! t o x i ; -1-- >1 i-2. Dy4 , 5 ag/kg 10/19/' toxi; -:ppb-ccv-u-i, s e e MeCH . t o x i ; *!" .... Blank-ll, SEE toxi;: t o x i ; :-RT2`.' t o x i ; '.a- - -S- a Blank-ll. SEE Blank-ll. SES Blank-12. SEE t o x i ; -Rs,,;;. :' .b-11. SEE toxi; : pb-11. SEE t o x i ; -r :s :: -2:jpb-11. SEE t o x i ; -r e .'K: -'.ppb-11. SEE t o x i ; :-R* 'l:. : ;ippb-ii, s ee t o x i ; :-r e -'K . -2 :!ppb-11. SEE t o x i ; ;-RES1C. -rCippb-ll. SEE t o x i ; '-R3J1C. :3ppb-11, SEE TOXI. -RSS10. - :.joppb-ll. s i e Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard Standard K>dV Ct 4a r t V n U k - 10 4 a n o i' i m nag 1.00 1.00 1.00 1 .0 0 1 .0 0 1.00 1.00 1.00 1.00 7.080 7.094 7.093 7.083 7.079 7.106 7.104 7.095 7.107 7.105 7.105 7.106 7.106 7.014 7.105 7.103 7.104 7.107 7.105 7.104 7.107 7.101 7.106 7.100 7.099 7.105 7.117 7.013 7.105 7.106 7.102 7.098 7.106 7.103 7.097 7.083 7.107 7.105 7.085 7.105 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 7.102 7.100 7.105 7.085 7.107 7.106 7.104 7.083 7.098 7.106 7.106 7.101 7.104 1064 bb 1185 bb 1198 bb 1222 bb 1311 bb 1493 bd 1689 bb 1526 bb 1402 NK 1774 bb 1625 bb 1335 bb 1369 bb 16S0 bb 1602 bb 1633 bb 1598 bb 1543 bb 1570 bb 1324 bb 1367 bb 1577 bb 1301 bb 1102 bb 1422 bb 1547 bb 1588 bb 1497 bb 1433 bb 1329 bb 1570 bb 1180 HM 1165 bb 1142 bb 1172 bb 1254 bb 1502 bb 1318 bb 1238 bb 1488 bb 1192 bb 1485 bb 1543 bb 1541 bb 1540 bb 1561 bb 1595 bb 1499 bb 1357 bb 1689 bb 1574 bb 1415 bb 1441 bb used. IA C 0.70 0.78 0.79 0.81 0-87 0.99 1.12 1.01 0.93 1.17 1.08 0.88 0.91 -30 -22 -21 -19 -13 -1 12 1 -7 17 8 -12 -9 1.11 1.06 1.08 1.06 1.02 1.04 11 6 8 6 2 4 0.88 0.90 1.04 0.86 0.73 0.94 -12 -10 4 -14 -27 -6 1.02 1.05 0.99 0.95 0.88 1.04 2 5 -1 -5 -12 4 0.78 0.77 0.76 0.78 0.83 0.99 -22 -23 -24 -22 -17 -1 0.87 -13 0.82 -18 0.99 -1 0.79 0.98 1.02 1.02 1.02 1.03 1.06 0.99 0.90 1.12 1.04 0.94 0.95 -21 -2 2 2 2 3 6 -1 -10 12 4 -6 -5 Soup 020199: Quantifia *. ar.: ?. .tel by laa on 10/19/99 j Tm -S I ' / l j / ' M T>. / * - / < / ' w*em i Soup 020199: Quantified u d printed by !* o 10/19/99 ri a XX eup 02019*: QaaaelCltf icintm* toy !* on 10/19/99 *e* 3 Soup 020199: Quantified nd vrlnted bjr in* oo 10/19/99 9ao 4 Ofiip 020199: Quantified ad print! toy la* on 10/19/99 Meche i Repace Mechel filebast r; .ied: Coippe :r. Print-.-- - ''-',3SL^ * -=t * oup-rats.pro\MethDB\101999b.adb 10:48 1999 ; ; -VA (. -- -c 2 - ;: s - u w Cotrpo ' 1 Name : Zncer -- Ref-: Queue -- Trece; Core, c: Standards; Ueer PT Value: User peak Factor: Incearste Wir.dtv Fect*r Chrom:-'-:?ra.-a m vir.c v: OAA (Chi) None ] .TC .ixed oooo oooo oooo o oo n oo & oo e & Reten:.." Time Imirc - Re la: ' .tenticr. ` RT Re - Time - :* (mini Peak re'.ecticn: -.133, Enabled .000, Disabled None ] .334 earest Respe - Tyr*: RefpO - ;: Polyn::- .al Type : . t Point c : Criin: Pic w-..;htin: Axis T.nsfci-raticn External reas linear 'xclude :/x lone Dnits: Pea/' - ' ----- a-'C --' Sm:ct ' Mir.dr - - Her.: ttunpe - --- Smcc: ; ---hod Join . -r/ cr-.reshold Reduc =.h--: ti-linj: Raise . maximum Draw De ce: She 1.1 '-3' : ' : .zti-z'.i Re :*: Abs:i Re :a:. AbSCl ?"' i.;s 5.3: nabled 3 .00 :o.oo .:o .00 '.:sabled ;o.oo SO. Disabled .00, Disabled ..oo, Disabled 00. Disabled t fojzaU i p f . f ______ i ro 1 O 2 o i "ft [ 1 M */*/** R er-rt H e th ti file : L a :c r c '.if i d = C c r p c .r.-i P r;n csd C . '.HASSLYT vied O c t 2. p r o s (c .:ed O c t 2 ' t u p - r a t s proX M athD B . 36:48 1999 ' : 10:55 1999 In :s: a - -- f ; Qu<?/ . ._ : . i c e Cert : : S tir.d ar C h r 3" : y r:-.- s t'.:. 70S (CU2 ) :one] . . 000000. 1.000000 .000 . 00000 D isab led - -- - . Tire Pe.-< S e '- i t t i e r . . 326. .coo, ..o n e ) .411 E nabled D isab led am t H eyy:- ete rn a l . a F it .'I .- .,: A x..; T r-r.z : -in e a r :< clude /X tn e O n :;: P e t c - : : - ---== S ir : c t i " ' M ir:.: / r Mur - = - - S ir: - * ... 6* " - - Rt R i. '.. - S 1- : - - - - - - - . - A h: : : ` - -' * 'n a b le d '..00 -.00 c a b le d 0.00 . . 50. D is a b le d . 00. D is a b le d . 0C, D i s a b l e d . 00. D is a b le d S y 02ol 11 " /t* H i . Me . t-M - .. . -*. Cc . Pr. ~ r..x a s s l y : '"< Cc: 2 - ?^SA r-c ~ 2 3UP-rats,pro\MethDR\101999b. mdb .}o :48 1999 1 :10: 56 1999 Cc- -- r.i : -re Ir r Ov. Cc-- cf Us.: 0* ` Ir. Ch. -* V- '.u-* >- - ` 5r - --- : ?rOSA lCta3) None] :ic ;oac. C ,.000000. Disabled ..000000 :.000 .00000a Re . Re : Ti" e RT - . T; - - ."3 pe- t '.*:-.icr. ' S7, Enabled .o:0. Disabled Nor.] .735 rue Re; : -5- "Yt* Re: : : . xcernal reu Pel yr. .rrua1 Tyy = Pc;-.: -i P:- *.v "; Ax: . -J- --- -* yinear xclude ./X one O n ;-. Ft. . - f : Sr: i: : M w - -: Sr- : . 'i ^ Jc . .- - -^ : Re - - Rr - - D-. ;-De Si ..... R At. Re . : At.- 1 =a i rabled o.oo .00.00 .00 -0.00 isabled 0.00 .50. Disabled .00. Disabled .00, Disabled .00, Disabled 1 Stfu-p O i f ? 7 lA S >Oi J > * H - M H H6&6B- m ib -s V "O * 4 ? pre\MthDBM01999b.adb /o f9 ? 7 Q uattro II, #6414E ` SOUP 020199: FACT Equipment Log 99092 PAGE 1/1 DATE: 10/19/99 ANALYST rrmnh STUDY NUMBERj m M l MATRIX: rat sera DESCRIPTION:Day? L4 FACT Method: ETS-8-51 Injection volume: 10 uL____ Cycle time: IQ milL- Electrode. Z-Spray--------- Mobile Phase: fAl? 0 mM NH4CH3C02 TN-A- or stndrd number (A) 99085-10-14----------- (B)JdsQH-------(B) TN-A-2997 Prepared (date/by): fAl 10/16/99 mmh________ (B) IQ/1^/99 sah Expires: (A) 04/00______________ (B)_2Qlfi--------- Store at room temp? @ or N Other:-------------------------------- --- Guard column: None_____________ _____ Part number: na_________ Lot number:jja. Analytical column: Keystone Betasil__________ ___________________ ------- Size: 2 x 50 mm________________ Type:_18----------------- Sphere size:J_um--------Part number: 055-701-2__________ Lot number: P9E11____ Serial number:0591804Z Analytical parameters: Drying gas (L/hrl: 350 ESI nebulizing gas (L/hr)_12___ Sheath gas (L/hr)_0 LC Flow rate: 300 uL/min. Back pressure: 65 bar HPLC solvent gradient: 10min-10-95 Time (min.)____ n o.oo______ 21 1.00______ 3)_i52_________ 41 7.50__________ 518.00____________ -$S_ 100 10 0 -210 910. 10JL Tuning Method Report Method: C :\HXSSLYNX\SOOT-RATS .PR0\ACQDDB\PF0S3 Printed: Tue Oct 19 15:40:03 1999 /O '/#*?? Page 1 MS SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. **S2 Set 3.00 40 5 0 2 150 250 Rdbk 3.01 -41 -8 150 251 Pressures Analyser Vacuum Gas Cell Rdbk 5.5e-5 4.1e-3 MSI LM Resolution HM Resolution Ion EnergyIon Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set Rdbk 14.0 14.0 0.9 0 .0 4 650 3 S e t Rdbk 14.0 14.0 10 2 .0 0 .0 40 0 650 8 38 1 Method: beet Modified: c'\jAMbnx\dOor-wits .prosnegro\io Fri Oct IS 11:15:03 1995 T M Oct 19 15:40.25 1999 -F T O d - P O k A - rfO J k -X J ' Solvent Deley ( a i m ) : 0.00 Function : 1 m Of 1 Mass Pair ( : Inter Channel Deley ( Secs ) : Spun < Daltons ) : Stert Tiae t Mine ) : End T i m ( Mine ) : Repente : Channel Parent Daughter 0.03 0.00 1 1 413-00 169.00 0.30 Com ( V ) IS Function : 2 ***** of 1 Mass Pair ( Inter Channel Delay 1: Secs ) : Span ( Daltons ) : Start T i m ( Mins ) : End T i m ( Mins ) : Repeats : Channel Parent Daughter 0.03 1 Dwell 1 499.00 99.00 0.30 cone < V ) <0 0 h \ Function : 3 *WI Pair ( Inter Channel Delay ( Secs ) : Span ( Daltons ) : Start T i m ( Mins ) End T i m ( Mins ) : Repeats : Channel Parent Daughter 0.03 10.00 Dwell 1 498.00 71.00 0.30 Com ( V ) CO Function : 4 W M of 1 m s s Pair ( Inter Channel Delay ( Secs ) : Span ( Daltons ) : Start T i m ( Mina ) End T i m ( Mins > : Repeats : Channel Parent Daughter 0.03 0.00 10.00 1 Dwell 427.00 80.00 0.30 40 Cone ( V ) 60 Masslynx - Sample List Sample List: C:\MASSLYNX\soup-rats.pro\SampleDB\101999b.SPL' Printed: Tue Oct 19 15:42:35 1999 / t Page Page Position: (1, Pile Name File Text MS File 1 101999012 MeOH Blank 2 101999013 MeOH Blank 3 101999014 MeOH Blank 4 101999015 TOX145-RBS10199-H2O Blank-11, SEE 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 5 101999016 TOX145-RBS10199-Sera Blank-11, SEE 10MIN-PFOS-POAA-PFOSA-IS 6 101999017 TOX145-RTS1 0199-Sera Blank-11, SEE 10MIN-PFOS-POAA-PFOSA-IS 7 101999018 TOX145-RTS10199-Sera Blank-12, SEE 10MIN-PFOS-POAA-PFOSA-IS 8 101999019 TOX145-RBS10199-5ppb-11, SEE 10MIN-PFOS-POAA-PFOSA-IS 9 101999020 TOX145-RBS10199-10ppb-11, SEE 10 101999021 TOX145-RBS10199-25ppb-11, SEE 11 101999022 TOX145-RBS10199-50ppb-11, SEE 12 101999023 TOX145-RBS10199-100ppb-11, SEE 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 13 101999024 TOX145-RBS10199-250ppb-11, SEE 10MIN-PFOS-POAA-PFOSA-IS 14 101999025 TOX145-RBS10199-500ppb-11, SEE 15 101999026 TOX145-RBS10199-750ppb-11, SEE 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 16 101999027 TOX145-RBS10199-1000ppb-11, SEE 10MIN-PFOS-POAA-PFOSA-IS 17 101999028 MeOH Blank 18 101999029 TOX145-RTS, 9R03230M, Dyl, Control,-10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 19 101999030 TOX145-RTS, 9R03231M, Dyl, Control,-10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 20 101999031 TOX145-RTS, 9R03232M, D yl, Control,-10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 21 101999032 TOX145-RTS, 9R03233M, Dyl, Control,-10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 22 101999033 TOX145-RTS, 9R03234M, Dyl, Control,-10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 23 101999034 TOX145-RBS10199-250ppb-CCV-11-1, SEE 10MIN-PFOS-POAA-PFOSA-IS 24 101999035 MeOH Blank 25 101999036 T O X 145-RTS, 9R03235M, Dy4, Control,-10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 26 101999037 TOX145-RTS, 9R03236M, Dy4, Control,-10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 27 101999038 TOX145-RTS, 9R03237M, Dy4, Control,-10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 28 101999039 TOX145-RTS, 9R03238M, Dy4, Control,-10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 29 101999040 TOX145-RTS, 9R03239M, Dy4, Control,-10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 30 101999041 TOX145-RBS10199-250ppb-CCV-11-2, SEE 10MIN-PFOS-POAA-PFOSA-IS 31 101999042 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 32 101999043 TOX145-RTS10199-250ppb-MS-11, 10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 33 101999044 TOX145-RTS10199-250ppb-MSD-11, 10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 34 101999045 TOX145-RTS, 9R03245M, Dyl, 5 mg/kg 10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 35 101999046 TOX1 45-RTS, 9R03246M, Dy1, 5 mg/kg 10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 36 101999047 TOX145-RTS, 9R03247M, Dyl, 5 mg/kg 10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 37 101999048 TOX145-RBS10199-250ppb-CCV-11-3, SEE 10MIN-PFOS-POAA-PFOSA-IS 38 101999049 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 39 101999050 TOX145-RTS, 9R03248M, Dyl, 5 mg/kg 10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 40 101999051 TOX145-RTS, 9R03249M, Dyl, 5 mg/kg 10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 41 101999052 TOX145-RTS, 9R03250M, Dy4, 5 mg/kg 10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 42 101999053 TOX145-RTS, 9R03251M, Dy4, 5 mg/kg 10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 43 101999054 TOX145-RTS, 9R03252M, Dy4, 5 mg/kg 10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 44 101999055 TOX145-RBS10199-250ppb-CCV-11-4, SEE 10MIN-PFOS-POAA-PFOSA-IS 45 101999056 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 46 101999057 TOX145-RTS, 9R03254-1M, Dy4, 5 mg/kg 10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 47 101999058 TOX145-RTS, 9R03254-2M, Dy4, 5 mg/kg 10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 48 101999059 TOX145-RBS10199-250ppb-CCV-11-1, SEE 10MIN-PFOS-POAA-PFOSA-IS 49 101999060 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 50 101999061 TOX145-RBS10199-H2O Blank-11, SEE 10MIN-PFOS-POAA-PFOSA-IS 51 101999062 TOX145-RBS10199-Sera Blank-11, SEE 10MIN-PFOS-POAA-PFOSA-IS 52 101999063 TOX145-RTS10199-Sera Blank-11, SEE 10MIN-PFOS-POAA-PFOSA-IS 53 101999064 TOX145-RTS10199-Sera Blank-12, SEE 10MIN-PFOS-POAA-PFOSA-IS 54 101999065 TOX145-RBS10199-5ppt>-11, SEE 10MIN-PFOS-POAA-PFOSA-IS 55 101999066 TOX145-RBS10199-10ppb-11, SEE 10MIN-PFOS-POAA-PFOSA-IS 56 101999067 TOX145-RBS10199-25ppb-11, SEE 10MIN-PFOS-POAA-PFOSA-IS 57 101999068 TOX145-RBS10199-50ppb-11, SEE 10MIN-PFOS-POAA-PFOSA-IS 58 101999069 TOX145-RBS10199-100ppb-11, SEE 10MIN-PFOS-POAA-PFOSA-IS 59 101999070 TOX145-RBS10199-250ppb-11, SEE 10MIN-PFOS-POAA-PFOSA-IS Masslynx - Sample List Sample List: C:\MASSLYNX\soup-rats.pro\SampleDB\101999b.SPL Printed: Tue Oct 19 15:42:35 1999 Inlet File Bottle Inject Volume SampleType Cone A 1 2 3 4 10min-10-95 91 10min-10-95 91 10min-10-95 91 10min-10-95 1 5 10min-10-95 2 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 10min-10-95 3 10min-10-95 4 10min-10-95 5 10min-10-95 6 10min-10-95 7 10min-10-95 8 10min-10-95 9 10min-10-95 10 10min-10-95 11 10min-10-95 12 10min-10-95 13 10min-10-95 92 10min-10-95 14 10min-10-95 15 10min-10-95 16 10min-10-95 17 10min-10-95 18 10min-10-95 41 10min-10-95 92 10min-10-95 19 10min-10-95 20 27 2289 10min-10-95 21 10min-10-95 22 10min-10-95 23 30 10min-10-95 42 31 10min-10-95 92 3332 10min-10-95 24 10min-10-95 25 34 10min-10-95 26 35 10min-10-95 27 36 37 10min-10-95 28 10min-10-95 43 38 10min-10-95 93 39 40 10min-1t>-95 29 10min-10-95 30 41 10min-10-95 31 42 43 44 10min-10-95 32 10min-10-95 33 10min-10-95 44 45 10min-10-95 93 46 10min-10-95 34 47 48 10min-10-95 35 10min-10-95 41 49 10min-10-95 93 50 5521 10min-10-95 1 10min-10-95 2 10min-10-95 3 53 10min-10-95 4 54 10min-10-95 5 55 10min-10-95 6 56 10min-10-95 7 57 10min-10-95 8 58 10min-10-95 9 59 10min-10-95 10 --1 0 --1 0 10 ---1 0 10 ---1 0 --1 0 --1 0 --1 0 --1 0 --1 0 . --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 . 10 -- 10 ---1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 --1 0 -- _ -- mmm mmm mmm mmm mmm """ "" _ _ MS M M SM SM SM SSMS. M M M SM SM Page 2 Page Position: (2,1) Masslynx - Sample Ust Sample List: C:\WASSLYNX\soup-rats.pro\SampleDB\101999b.SPL` Printed: Tue Oct 19 15:42:35 1999 File Name File Text 60 101999071 TOX145-RBS10199-500ppb-11, SEE 61 101999072 TOX145-RBS10199-750ppb-11, SEE 62 101999073 TOX145-RBS10199-1000ppb-11, SEE / V 997 Page 3 Page Position: (1, 2) MS File 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS Masslynx Sample List Sample Ust: C:\MASSLYNX\soup-rats.pro\SampleDB\101999b.SPL' Printed: Tue Oct 19 15:42:35 1999 Inlet File Bottle Inject Volume SampleType Cone A 60 10min-10-95 11 61 10min-10-95 12 62 10min-10-95 13 10 -- 10 -- 10 -- -- -- -- Page 4 Page Position: (2, 2) Date: Data Analyst FACT: DATA REVIEW SUMMARY FORM ' Data Review Sign-Off Analyst Review Name /Date: T** ;. Iof 2 \Ac l/jr/ FACT Study #: T>t tf% Matrix/Timepoints: TZJ-tra. Sample List -hty * I Technical Review Nome / Date: . Quality Assurance Review N o m e /D a te :____________ i Set-up Analysis Date/Analyst Instrument fo /zi/tf 3+S AhJ . o iz m Data Entry: t o d e n l t f t A Comments / Justifications: MU. L y rA ia fv fta IM- 0 Hirfa ^ Th. nuts L u-vir*. tu r- U tlL .____________ LOO: yWd RA2: Ad" Retraction Bionic f(A Matrix Blank AM Calibration Checks: / / 4 ________________ MS/MSD: tf-trtA Do)- f , n W l lie . S ^ j.L t f l 4*r TqAA , /s t/ztSuJ -Per 7pro- otu>-ls ____ --- V t.b n .lra * . - h t- tS A k J & *-C- J o b _______ xL J J ru>-l b- W (M tr--------------- je k s J-se^oit.iullj kttre. SULfl /'*- -fit. 7>AA 'P't-U* l--J d Lt rtuxs-lij& b/ ~~T*rS lojzS'Jtir------- Analyte: C cH z) Acceptable Linear Range: f - P f r h -- LOQ: _ P f f L R-2: 0-1?T2-?S Extracted Blank: / p . jU * lt)Q Matrix B I o n i c jU tt, LQ. M LCalibration Checks: MS/MSD: kVPjtvA Vo rtflA L u ______ \A L ^-4 ^ a5 ^ Data Status: Analyte: TF06A C C d 'f' '^ Acceptable Linear Range: j-Pjfl -- ------------- LOQ:____ f ^ k ____ Extracted Blank: f&c -fhn-LoQ . RA2: 0 ? fV 5 i> _ Matrix Blank: C&s lU * . Ld(k MCalibration Checks: MS/MSD: )uA 4o _______ ~j 1AL Data S itu s:______________ ^ mm^ m __ C t / t b i - h * - / jh e J c s J * r f F S ___________ 4 J J . 4 - f to S a x jte / 4 ia J - iK ied/or-s - f i t t e d r C o-/ chc& flU -I !*Jc d stu*L. T u . e, P i n i tuer*- Jvtytu d ~A "PyOi/u. &^Jqm/ -fri lo lU 3tU~j-L <t>er/ 4* h - K .f i C u m /t b lin d s i 4 3 > " /o K - J e m d - t a i * - . 4 4 A o t s * J * tK jb d / d j) -fit. Iniutv ho\*M f t-- ~HtL. Hudit [Jeudi LtJrf s. less dU-^._ lU LOQ. hJ^Kj IU, h k j t r t-ej b f _ o r < k c . Jel/igJuj ,^v S5 d vrr- d0 JUUr'' puT to iK tU ) * - d i* -- tir jlte . ( j/d ) G s ^ s -r / r - r 7 tir s ,* + Y > L < r s e - K /e & f5 = ^ F * ? /iL C H e z * . fZ /L ir - e t? /v < & ~ , , ij l U irn ttoU *? Ali.. , i i c u i t U tk d AK " "d ^ f .- t mJt-Kvj t e e fe ""* ,, Date: Data Analyst: FACT: DATA REVIEW SUMMARY FORM Us_______________ ______ Data Review Sign-Off Analyst Review Name / Date: , tjz s h 'j fgt 3 pf 2 lA t loH i \ FACT Study H: Matrix/Timepoints: Sample List: 7 _____________________ __________ U 4 . esHntn 0/ o i L Z - ? ? ^ _____________________________________ _______ Set-up Analysis Date/Analyst /y a a /ff Instrument: nL z S * i Analyte: C b ) Acceotable Linear Ranae: LOO: Ma R"2: MA MA Extraction Blank: Mfir Matrix Blank: Ma Calibration Checks: MA MS/MSD: --- - Data Status: Technical Review p , N am e/ Date: A t W - to Quality Assurance Review Name / Date:___________________________ Data Entry: AjttV - YUlA 4 o r M ^ J j it, (JC , Comments /Justifications: ____________________________ lO /ji/t pedes vere.__- A f f i L - Il & Z S T : s L t d / Le. G> TZ- f 3 jj> lJ -Z * '-A s/ft a * -d f a. ?L Y!U* f 2> ot V e r e . J ta j+ e e f A _________ A Ac-Drat*J . LoJ fj/UA*' a*-*V<L 44~ SZuHfh S e f. "%* C d eLck-S 4 jfeJ \ /pnlja-Llu (Ill- 4a /a-cJc 3 Sim ple. 'OJLr ' A M tTM ~A " '/ l/ * " ? } ~ 4 L b ci& neej 0-nrf JL -'-// / H\J f4 `Or<1 4 U * r/&5 i f 9________________ _ 35J S r e a . C a e t u b f o h f P o is ts lc u - f /h . 4 u C * .n * S 2 Caf-cbe/ci 5 * - y b J LT J r/J-4j1 kjtre /u 4 te* j> b J U /,4b 7S - 'U s 'a/z*/f<r S*~pl*S s b u f j L tat-yXirCr^ du*, -b "fL. d b 'L J 4 ebeke- 7L >Li yt br&cb-led Ltj 4L. CtUtlrCS f ? ,4 s(*> *-1*4.* j (5) C *JebeL doV idl/is Ky* 4Le>Uk4 4a u t* r ts S J 4 ^ I s s i 4 Sa^plt, b*d~ A6_______ Qu'eu. Cau.*4 s L i q> J ( J 4 . 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W O \ W l * "'10" " * Job Cod: printed: n Oefc 2 S S . e x p o u n d 2 : PTO8 (Ch2) Typ* 9 MaM 1 102299001 la^laliat t t MaOH Blank 2 102299002 3 102299003 4 102299004 5 102299005 6 102299006 7 10229900 8 102299008 9 102299009 10 102299010 11 102299011 12 102299012 13 102299013 14 10229901 15 102299015 16 102299016 17 102299017 18 102299018 19 102299019 20 102299020 21 102299021 22 102299022 23 102299023 24 10229902 25 102299025 26 102299026 21 102299027 28 102299028 MaOH Blank ,, ,rr t o x u s -r b s i o i -i c o s" rE Toxi4S-RBSioi-s.n> " -}? ?" TOXH5-RTS101-S.ru Blk-12. SEE Standard T0XH5-RB31019-SPP<>-12" SEE TOXM5-R*S10l9-lOl>PO-;2. SEE Standard Standard TOXH5-BS10l99-25ppb-12- SEE TOXlkS-RBSlOlSB-SOppb'l2- SEE TOXlS-W>S101-10PPb-l|- oe Toxi4S-asiom-25oppb-|' see TOX14S-RS10l9-S0OppP-;2- SEE Standard Standard Standard Standard Standard Standard 5 r - ^ " :i o X p b - l i . S" O50-a*tl0/19/99 t S i45~RTS_9E0324SK# W y l . / g D50-*tl0/19/99 T0X14S-ETS-9E03244M. Dyl. W J ' DS0-*Xt10/19/99 TOX14S-RTS-BR0J24TO. D.yl. W g ' D50-axtl0/19/99 TOX145-ET5-9E0324O4. Dsyl. ,,D50-Xtl0/19/99 TOC145-RTS-9R03249I4. Dyl. T0X14S-RBS101*-2S0j>pb-CCV-ll 1. SEE QC H*0H Blank D50-xtl0/19/99 IOX34S-RT5-9R032S. By*. g j ' g ' 10/19/99 TOX14S-RTS-9R032S1M, 0y4, E 50.C 10/19/99 TOX14S-RTS-9R032S2M. D.y4. ,, 50- 10/19/99 TOX145-RTS-JR032S4-W. M y 4 . g g 050- 10/19/99 TOX145-RTS-9R03254-M. Ojy4. S M / 9- TOX145-RBS10199-250ppb-CCV-ll 2. SEE 29 102299029 30 102299030 31 102299031 32 102299032 33 102299033 3 10229903 35 102299035 36 102299036 37 102299037 38 102299038 39 102299039 40 102299040 41 102299041 MaOH Blink ,,r TOX14S-RBS10199-H2O R1^ 12' 3" TOX14S-RBS10199-S.ru. Blk-12. SEE TOX14S-RTS10199-S.nl. Blk-12. SEE TOX145-RBS10199-SPPB-12, SEE TOX145-RBS10199-- 10ppb-12, SEE T0X14S-RBS10199-2Sppb-12. SEE TOX14S-RBS10199-5Oppb-12. SEE TOX14S-RBS10199-100ppb-12. 5EE TOXl45-RBS10199-2S0ppb-12, SEE TOX14S-RBS10199-- SOOppb-- 12. SEE TOX14S-RBS10199-- 7S0ppb-12, SEE TOX14S-RBS10199-- 1000ppb-12. SEE Standard Standard Standard Standard Standard Standard Standard Standard Standard BT 7.190 7.183 7.196 7.170 7.162 4.93 9.76 24.80 49.30 97.60 248.00 493.00 735.00 976.00 7.171 7.176 7.184 7.173 7.164 7.166 7.169 7.169 7.179 7.172 7.169 7.173 7.143 7.168 7.161 7.168 7.165 7.168 7.172 7.168 7.164 7.169 7.170 7.171 7.165 7.172 7.163 4.93 9.76 24.90 49.30 97.60 248.00 493.00 735.00 976.00 7.169 7.173 7.19 7.169 7.173 7.189 7.171 7.169 7.175 ATM 119 82 Cene, fia Dav 0.24 < 0.00 94 112 0.08 MK 88 0.00 MK 263 330 528 1195 1909 5512 11228 22030 28219 36823 3.4 bb 4.94 bb 9.34 bb 24.22 bb 40.12 bd 120.40 bb 247.73 bb 499.41 bb 626.31 bbX 018.00 bbX 0 -4 2 -19 23 -0 -1 -15 -16 109 0.01 M4 4125 9.49 bb 6459 141.49 bb 5637 123.18 bb 3710 0.23 bb 4390 169 95.16 bb 1.33 bb -99 40 0.00 MM 4350 94.50 bb 4238 92.01 bb 6453 141.35 bb 5257 114.70 bb 4193 217 23 91.01 bb 2.42 bb 0.00 KM -99 75 0.00 MH 96 0.00 KH 262 336 521 1235 2005 5514 11233 21189 29094 37681 3.43 bb 5.07 bb 9.20 bb 25.11 bb 42.26 bb 120.43 bb 247.86 bb 469.68 bb 645.81 bbX 837.11 bbX 3 -6 1 -1 23 -0 --S -12 -14 ilia 062498: Quantitt** Print* by l " 10/29/99 Quantify Compound TQX145-rt art dilution*, day X 6 4- t 10/1/* *** ~ " o<Ufxl: Mon Oct 25 0:2.:5S Job Cod: Pnntad: Mon Oct 25 05:55:42 1555 confound 2 : PFOSA ICh4) typ HIM 1 102299001 2 102299002 3 102299003 4 102299004 5 102299005 6 102299006 7 102299007 B 102299008 9 102299009 10 102299010 11 1 0 2 299011 12 1 0 2 299012 13 102299013 14 102299014 ftaaplaliat Tat M0H Blank MaOH Blank T0X145-RBS101S5-H2O * " " ' * " _ O X 14S-RBS101S9-STM B U -1 2 . TOXHS-RTS10155-Snni 5It TOX145-RB5101S9"5ppb-12, SEI TOX145-RBSlOl99-10ppb-12, SEE TOX14S-BBS10199-25ppb-12. SEE T O X 1 4 5 -R B S 1 0 1 9 9 -5 0 p p b -1 2 , SEE tO X 1 4 5 -R B S 1 0 1 9 -1 0 0 p p b -1 2 , SEE T O X 1 4 $ -R B S 1 0 1 9 9 -2 S 0 p p b -l2 , SEE T O X 1 4 S -R B S 10199-500ppb-12, SEE T O X 145-R B S 1 0 1 9 9 -7 S 0 p p b -1 2 , SEE T O X 1 4 5 -R B S 1 0 i 9 -l0 0 0 p p b -1 2 . SEE Standard Standard Standard Standard Standard Standard Standard Standard Standard 15 102299015 16 102299016 H*0 Bl a n k W k Q , D50-axt 10/19/99 TOX145-BTS-9B0J245K, Dayl DSO-axtlO/19/99 p 102299017 IB 1 0 2 299018 19 102299019 20 102299020 21 102299021 SK K SK SSffi g : g g : S s k k s SUKr-XSUiS: Z& TOX145-RBS10199-25Oppb-CCV-ll-l, SEE 22 102299022 23 102299023 HaOH B la n k nso-xtl0/19/ TOXUS-RTS-9R03250M. B.4, 5/XQ. 10/1.9/99 24 102299024 25 102299025 SiESr-i: : 26 102299026 27 102299027 2B 1 0 2299026 29 102299029 30 102299030 31 102299031 32 102299032 33 102299033 34 102299034 35 102299035 36 102299036 37 102299037 36 102299038 39 102299039 40 102299040 41 102299041 sssk sse s g ; a s- TOX145-BS10199-25Oppb"CCV-ll-2. 5E*. HaOH B la n k TOX 145-RBS10199-H2O Blk-12, SEE TOXl45-RBS10199-Srun Blk-12. J" TOXI45-RTS10199-Saru Blk-12, SEE TOX145-RaS10199-5ppb-12, SEE TOX145-RBS10199-10ppb-12. SEE TOX145-RBS10199-25ppb-12 SEE T O X 1 4 5 -A B S 10199-50ppb-12, SEE T O X 145-R B S 10199-10O ppb-12, SEE T Q X 14S-R B S 10199-250ppb-12 SEE T O X 1 4 5 -R B S 1 0 l9 9 -5 0 0 p p b -1 2 , SEE T O X 1 4 5 -R B S 1 0 1 9 9 -7 5 0 p p b -1 2 , SEE T O X 1 4 S -R B S 1 0 1 9 9 -1 0 0 0 p p b -1 2 , SEE Standard Standard Standard Standard Standard Standard Standard Standard Standard KT 7.64 6 7 .6 4 0 7 .6 4 3 7 .8 5 0 7 .6 4 3 4 .9 3 9 .7 7 2 4 .6 0 4 9 .3 0 7 .6 2 6 7 .8 3 4 7 .8 4 0 7 .8 2 8 9 7 .7 0 24B .00 4 9 3 .0 0 7 3 6 .0 0 9 7 7 .0 0 7 .8 2 1 7 .8 2 0 7 .8 2 6 7 .6 2 6 7 .6 3 5 7 .8 5 3 7 .8 2 5 7 .6 2 6 7 .8 2 5 7 .8 2 5 7 .6 4 2 7 .8 2 4 7 .6 6 8 7 .6 4 6 7 .8 3 3 7 .6 4 6 7 .6 4 5 7 .6 5 0 7 .8 2 8 7 .8 5 2 7 .8 4 6 7 .8 5 3 7 .6 4 3 4.93 7.826 9.77 7 .8 2 7 2 4 .6 0 4 9 .3 0 9 7 .7 0 2 4 8 .0 0 4 9 3 .0 0 7 3 6 .0 0 9 7 7 .0 0 7.851 7 .8 2 8 7 .6 3 0 7 .8 4 6 7 .8 2 6 7 .8 2 7 7 .8 3 2 A r*a C a n e . P la a %Dv 465 4 .2 3 bb 331 3 .4 2 bd 152 2 .3 3 MM 151 2 .3 3 MM 95 615 1344 3615 5624 16036 39992 16266 126147 170969 1 .9 9 MM 6.36 bb 9.57 bb 23.35 bb 35.54 bb 110.68 bb 244.14 bb 5 3 7 .2 5 bdX 7 6 7 .0 3 bbX 1 0 3 9 .1 9 bbX 29 -2 6 -28 13 -2 9 4 6 424 3 .9 8 bb 1404 9.94 bb 2212 14.13 bb 1199 8.69 bb 1612 11.19 bb 1370 216 9.72 bb 2.73 bb -99 37 1 .6 3 bb 330 3 .4 2 MM 316 3 .33 bb 398 3.82 bb 422 3 .9 7 MM 337 283 3.46 bb 3.13 bb -99 25 1.56 bb 61 1 .7 8 M4 47 1 .7 0 MM 56 730 1319 3425 5469 18963 41057 88564 125699 168896 1 .7 5 MM 5.64 bb 9.41 bb 22.20 bb 34.60 bb 116.50 bb 250.60 bb 5 3 8 .9 3 bbX 7 6 4 .3 1 bbX 1 0 2 6 .4 9 bbX 19 -4 -10 -30 19 1 9 4 5 ,ll* 0624*8 : Quntltat*d and Printed by la* 10/25/* hir <a a S 2222 oooo o -0-4<'4M00<-I'4~If-.-I o o o o o o 2 2 g ;8 OO O OOO 2 -aOa- Qa PxZ? '9 aA '0 'a0 in3 rtOOOOOOw^., no^ivntoorffH'Vvii^noans-iofo'AMNNNNNNNNnnn b r- r* o o o Ol o o a S a S <a<eM tr* OBCOOHOOOOt A A O B iffiO O O O O O O l Kt * iss s/et/ot 3e 3c 3c e 3S 3 5c 3c e3 o v v o v v o v o U U U U U U U U it lbli*4m4M Wi <Jl Ui W!*J nnn nn nn w n AAAAA SSSNS ooo e o OOOOO Ui>u u u *X X K X 3 <oQtnQo<iQnoinDnoQi)Mloii g U U U WU lUd UU MU lH i4tHi inSi u Mu n v i M H (1 I I M . r4 If j Iin 4 Jt I S O OOQO <n<no O O O . >u %. Mo M 0M O 9 ON N ll iir .J II) . . M U Id 3 3 3 3 3 N N U I I U M V) V) V) (0 x r f u n n n r NNNf ... . . i Afib i AAaaa-aa j'>**a*a" a'*'a*'a*' *a (a o I I I f_ai&_oama_oo_ooAoO_cort o o 3 3 3 a" h n* a* Hh nN i *X- x><>i>t >0 33333 SSESX3 3.3.3.33 5 sssi 4 VS t3OMS AASN NNM -I I I i-4 >a a & &8- s S i i l i !o w bi n o o_ *i1O <fi o 33 -NlflfM lOOppl * i >Si A A NNNNN I . . II II M Al t 9> *91> " OOO o o o o o o o o c AAAA< O O O O O* AKAK AK KK0^ AFO-.A--O S Si S S S S oo ooo IMKMM VI M M VI 3333: s s i s 4iIddF-Bd-iIi<nnIi nmi D i i n i n i n i n i n < / i i / ) < / ) S i n i Av i i Ai Ai i ) t f i / > i / i d i Oi Ai AS i / i d i A^) Ad i n i i ) A^i i i lllliiliilllliiiiiliiliiil lll ll lll O OO O + -F h h rtn r4N r o o o o ow ow rw O O O A AA ~ ' ooooooooooooc 'S I I W M N N N f li f4lA4A4A4A4A4A4ai aA44AA44 J O O O O O QO OO O O O O O t o o <A(A ^A A Sa4A4A<A A A4Av A4P 4 AI A4 A4 A4 AI A4 A4 A4 A4 A4 A4 A4 3000000000000 O O O o OO i 3+c* 1 ! 3 3 i I i . QC249C: Q o a a tl t t l a d m a u d h 1 1 0 /2 / Quantify Calibration M p o r t T0OXX1I4OS--rraat m#oiruwn dimluution#, 4--Y' 1- Compound 2 name: W*OS . 1 0 /1 9 / *BK gS5K 2SSSSfxV !S51 Weighting: 1/x, Ante dans: None A ^Q #A_ Response- 0 0 X/ mo ,lia O<240: Quantitatod and Tintod by id* 10/23/ ______ _________ ______________________________ _-- Cone 40h-0 ' 600.0 800- ____________ TOX145-rC s a r w **-- -- * -- - ICompound 3 name: PFOSA Coefficient of D etraction : 0.989156 Calibration curve: 164.764 x + -232.515 W e i g h t l/x . A xis 1.71e5n Non. : Response- / I -233-*- 0.0 200.0 t-.it 0C24M: Quantitatad and Frtntad toy iaa 10/25/ 400.0 600.0 800.0 Cone . day 1 t i - . 10/1/ * Compound 4 name: IS (C h i) Response Factor: 2692.44 Response type: External Std, Area Curve type: RF 3.07e3 Pig* 4 X Response- / / /' / / / 0 AMlia 0C 24M : Quantitytad and fTintad b y i " 1 0 /2 S /M ------ Cone Method Report Method file: test modifid: Compound : C: V H St X \ -- U . - r . t , i 0 ' " > ' D M 0 2 2 9 . . Men Oct 25 06:39:55 1999C 2: Pros ICh2) Compound Nemo: Internel Ref.: Quantify Trece: Cone, of Standard*: User RF Value: UJtr Peak Faetor: Integrate Window rector: Chromatogram mass window: Peek Location Retention T i m m m ) : Relative Retention Ti m : RT Reference: Tine Window m m : peak Seleccin: Reaponae Reaponse Type: Reaponae: calibracin Curre Polynomial Type: point of Origin: Flt weighting: Axis Transformaron: Concentration Unit: Noise p*ak-to-peak amplitude: Smooth Smoothing: Window size mean*) : Nuaber of smooths: Smoothing method: Baaellnes Join valley threshold: Reduce peak tailing: Raise baseline maximum: Peak Separation Draw vertical threshold: Detect snouldecs: Shoulder threshold: Reaponse Threshold Relative height: Absolut* height: Relative area: Absolut* area: pros (Cb2) (None] TXC Cone. A 1.000000, Disabled 1.000000 2 .0 0 0 l.OOOODa 1 .178, Enabled 0.000, Olsabled (None] 0.262 External Areas Linear Exclude 1/X None 2300 Disabled 2 30.00 2 0 0 .0 0 5.00 90.00 Disabled 30.00 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled Paq 2 3 M 1 X -XA Method Report Method file: Lest modified: Compound: Printed: C -\H A 3S L 'f7\em elia-rats.P A O \H ethD B \102299e.m db Hon Oct 25 06:39:65 999G 3: prosA IC M ) Mon Oct 25 01:02:23 1999 Compound Heme: Internel Ref.: Quantify Trece: Cone, of Stendardi: User RF Velue: User Peek Factor: Integrate Window Factor: Chromatogram mess window: Peek Location Retention Time (mins): Relative Retention Time: RT Reference: Time Window (mins): Peak Selection: Response Response Type: Response: calibration Curves Polynomial Type: Point of Origin: n t Weighting: Axis Transformation: concentration Units: Noise Peak-to-peak amplitude: Smooth Smoothing: Window size (scans): Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: Peak Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative area: Absolute area: PFOSA (CM) (Hone) TIC Cone. B 1.000000, Disabled 1.000000 2 .0 0 0 l.oooooe 7.146, Enabled 0.000, Disabled (Monel 0.273 Nearest External Areas Linear Exclude 1/X None 161 Enabled 2 1 30.00 200.00 5.00 90.00 Disabled 30.00 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled Page 3 o I t 2 * f ijis h ? Method Report Method file: Lest Modified: Compound : printed: C: \KWSLYWC\eell.-rt..PRO\M.thDB\10229e .mOb 4: IS (Ch3> Mon Oct 2S 0^:03:23 Compound Name: Internel Ref ' Quantify Trace: Cone, of Standard*: User RF Value: User Pea* Factor: Integrate Window Factor: Chromatogram mass window: Peak Location Retention Time lm*l : Relative Retention Time: RT Reference: Tiae Window (am*) : Peak Selection: Response Response Type: Response: Calibration Curves Polynoadal Type: point of Origin: Fit Weighting: Axis Transformation: Concentration XS (Ch3) (None) TIC rixed l.oooooo. Disabled 1.000000 2 .0 0 0 l.OOOODa 7.040, Enabled 0.000, Disabled (None] 0.239 Nearest External Areas Linear Exclude 1/X Hone Units: Noise peak-to-pea* amplitude: Smooth Smoothing: Window site (scans) Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: Peak Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: ResDonse Threshold Relative height: Absolute height: Relative area: Absolute area: Disabled 2 30.00 200.00 5.00 90.00 Oisabled 30.00 1.50, Disabled o.oo, Disabled 2.00, Disabled 0.00, Disabled Page 4 3 * * l'l-n fo A M E LIA 062498: F A C T E q u ip m en t Log 99114 Q uattro n , #6448E PAGE DATE: 10/22/99 ANALYST: ias NUM BERJffitM L-M ATRK R ^ D E S C R IP I10 N i D! iaM J!ESEM FACT Method: ETS-8-5.1 Injection volume: 10 uL_ Cycle time: 10 min. Electrode:J^Sprai^ Mobile Phase: rav? nmMNH4CH3C02 TN-A- or stndrdnumber (A) 04085-10-14 Prepared (date/by): fW 10/16/99 sah _ _ Expires: (Al 04/00__________ __ (B)MeOH (B! TN-A-2945 m i 10/20/99 ias (B) 04/00 Storeatroomtemp? 3 or N Other. Guard column: None Partnumber: na____ Lot number: na Analytical column:JCeystoneBetasil------------- ------------- Size: 2 x 50 mm_______ ______ Type._C18_--------Part number: 055-701-2__________ Lot number: P9EH Sphere size: 5um____ Serial number.0591816Z Analytical parameters: I*m 8g(U M K 300_ ESI nebulizinggas (L/br)J0----- Sb=h g* (U b.)i LC now rate: 300uLAnin. Backpressure: 62bar_ HPLC solvent gradient: 10min-10-95 Time (min.) 1 ) 0.00 2 ) 1.00 3) 5.50 4) 7.50 5) 8.00 %B 10.0 10.0 95.0 95.0 10.0 T a p in g M ethod R e p o r t M ethod: C: \M A SSL Y K X \A M E L IA -R A T S.P R 0\A C Q U D B \P F 0S 1-6K V Printed: Fri Oct 22 09:58:58 1999 Page 1 SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. S et Rdbk 1.60 40 5 0.2 150 250 1.60 -14 "4 149 253 Pressures Analyser Vacuum Gas Cell Rdbk MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier S et Rdbk 15.0 15.0 2.0 0 .0 4 650 1 MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier S et Rdbk 14.0 14.0 10 2.0 0 .0 40 0 650 41 38 40 Scanning Method Report S o lv e n t D aisy ( ** > 0.00 fu n c tio n : 1 m m of 1 Maso fait < Intar Channel Delay ( Secs ) : Span ( Daltons ) : Start Tine ( Kins ) : End Tlae ( Mins ) : Repeats : Channel Parent Daughter 0.03 0 .0 0 0 .0 0 1 0 .0 0 1 Dwell (Secs) Coll E n e r g y <*V) 413.00 169.00 0.30 30 Cone ( V ) IS function : 2 M M of 1 Maas Pair ( ESP- ) Inter Channel Delay t Secs ) : Span ( Daltons > : Start Tlae ( Mins ) : End Tlae ( Kins ) : Repeats : Channel Parent Daughter 499.00 99.00 0.03 0 .0 0 0 .00 1 0 .0 0 1 Dwell 0.30 (Secs) Coll E nergy <eV) 45 Cone ( V ) SO fu n c tio n : 3 M M of 1 m o e *!' < U F ' ) Inter Channel Delay ( Secs ) . Span ( Daltons ) : Start Tiae ( Mins I : End Tiae ( Mins ) : Repeats : ,,, Channel Parent Daughter 0.03 o.oo 0.00 10.00 M 11 (Sacs) coll m . t g y I.V) . m o d 10.00 Cone ( V ) CO fu n c tio n : 4 M M of 1 Masi Pair C **" > Inter Channel Delay ( Secs l : Span ( Daltons ) : Start Tine ( Hina ) : End Tine ( Mins ) : Repeats : w Channel Parent Daughter 0.03 0.00 0.00 10.00 Dwell (Secs) Coll Energy (eV) 499.00 0.40 45 Cone ( V ] 60 g* 1 Method Report Method File: Last Modified: Printed: c :\m a s s ly n x \a m e lia -ra ts .p ro \a c q u d b \1 0 m in -i-95 F rid a y , O ctober 22, 1999 0 9 :5 6 :3 6 Friday, October 2 2 , 1 9 9 9 0 9 : 5 9 : 2 5 HP1100 LC Pump Initial Conditions Solvents A% B% C% D% Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 9 0 .0 10.0 0 .0 0 .0 0.300 10.0 0 400 30.0 30.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 5 entries which are Time 0.00 1.00 5.50 7.50 8.00 A* 90.0 90.0 5.0 5.0 90.0 B% 10.0 10.0 95.0 95.0 10.0 C% 0 .0 0 .0 0 .0 0 .0 0 .0 D% 0 .0 0 .0 0 .0 0 .0 0 .0 Flow 0.300 0.300 0.300 0.300 0.300 Pressure 400 400 400 400 400 HP1100 LC Pump External Event Timetable The Timetable contains 3 entries which are Time initial 0.00 0.10 Column Switch Contactl Off Off Off On Off Off Contact2 0" On Off Contact3 Off Off Off Contact4 Off On Off HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (|il/min) Draw Position (mm) Stop Time (mins) Injection Volume ((il) Vial Number 200.0 200 0.00 9.00 10.0 13 Masslynx - Sample List Sample List: C:\MASSLYNX\amelia-rats.PRO\SampleDB\102299a.SPL Printed: Fri Oct 22 09:58:46 1999 Page 1 Page Position: (1,1) File Name File Text MS File 10MIN-PFOS-POAA-IS-PFOSA 1 102299001 MeOH Blank 10MIN-PFOS-POAA-IS-PFOSA 2 102299002 MeOH Blank 3 4 102299003 TOX145-RBS10199-H2O Blk-12, SEE 102299004 TOX145-RBS1 0199-Serum Blk-12. SEE 5 102299005 TOX145-RTS10199-Serum Blk-12, SEE 6 102299006 TOX145-RBS10199-5ppb-12, SEE 7 102299007 TOX145-RBS10199-10ppt>-12. SEE 8 9 102299008 TOX145-RBS10199-25ppt-12, SEE 102299009 TOX145-RBS10199-50ppb-12, SEE 10 102299010 TOX145-RBS10199-100ppb-12, SEE 11 102299011 TOX145-RBS10199-250ppb-12, SEE 12 102299012 TOX145-RBS10199-500ppt>-12, SEE 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 13 102299013 TOX145-RBS10199-750ppb-12, SEE 14 102299014 TOX145-RBS10199-1000ppb-12, SEE 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 15 16 17 18 19 20 21 102299015 102299016 102299017 102299018 102299019 102299020 102299021 MeOH Blank TOX145-RTS-9R03245M, Day1, 5mg/kg, D50-e>rt10/ 9 99 TOX145-RTS-9R03246M, Day1, 5mg/kg, D50-ext10/ 9 99 TOX145-RTS-9R03247M, Day1. 5mg/kg. D50-eJd10/19/99 TOX145-RTS-9R03248M, Day1, 5mg/kg, D50-ext10/19 99 TOX145-RTS-9R03249M, Day1,5mg/kg, D50-ext10/19/99 TOX145-RBS10199-250ppb-CCV-11-1, SEE - 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 1 0 MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 1 0 MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 22 23 24 25 26 27 28 102299022 102299023 102299024 102299025 102299026 102299027 102299028 MeOH Blank TOX145-RTS-9R03250M, Day4,5mg/kg, D50-ext10/19/99 TOX145-RTS-9R03251M, Day4. 5mg/kg, D50-ext10/19/99 TOX145-RTS-9R03252M, Day4, 5mg/kg, D ^ x t1 0 /1 9 /9 9 TOX145-RTS-9R03254-1M, Day4, 5mg/kg. D 50-10/19/99 TOX145-RTS-9R03254-2M, Day4. 5mg/kg, D50-10/19/99 TOX145-RBS10199-250ppb-CCV-11-2, SEE 10MIN-PFOS-POAA-IS-PFOSA 1 0 MIN-PFOS-POAA-IS-PFOSA 1 0 MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 29 102299029 MeOH Blank 30 102299030 TOX145-RBS10199M-I2O Blk-12, SEE 31 102299031 TOX145-RBS10199-Serum Blk-12, SEE 32 102299032 TOX145-RTS10199-Serum Blk-12, SEE 33 102299033 TOX145-RBS10199-5ppb-12, SEE 34 102299034 TOX145-RBS10199-10ppb-12, SEE 35 102299035 TOX145-RBS10199-25ppb-12, SEE 36 102299036 TOX145-RBS10199-50ppb-12, SEE 37 102299037 TOX145-RBS10199-100ppb-12. SEE 38 102299038 TOX145-RBS10199-250ppb-12, SEE 39 102299039 TOX145-RBS10199-500ppt>-12, SEE 40 102299040 TOX145-RBS10199-750ppb-12, SEE 41 102299041 TOX145-RBS10199-1000ppb-12, SEE 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA lOMIN-PFOS-POAA-IS^PFOSA 10MIN-PFOS-POAA-IS-PFOSA M asslynx- Sample List Sample List: C:\MASSLYNX\amelia-rats.PRO\SampleDB\102299a.SPL Printed: Fri Oct 22 09:58:46 1999 Page Position: (2. 1) Inlet File Bottle Inject Volume Sam ple Type C one A C oncB C oncC C one D C one E C one F 1 10min-10-95 91 2 10min-10-95 91 3 10min-10-95 1 4 10min-10-95 2 5 10mirv10-95 3 6 10min-10-95 4 7 10min-10-95 5 8 10min-10-95 6 9 10min-10-95 7 10 10mir>-10-95 8 11 10min-10-95 9 12 10min-10-95 10 13 10min-1O-95 11 14 10min-10-95 12 15 10min-10-95 92 16 10mir>-10-95 13 17 10min-10-95 14 18 10min-10-95 15 19 10min-10-95 16 20 10min-10-95 17 21 10min-10-95 33 22 10min-10-95 92 23 10min-10-95 18 24 10min-10-95 19 25 10min-10-95 20 26 10min-10-95 21 27 10min-10-95 22 28 10min-10-95 34 29 10mir>-10-95 93 30 10min-10-95 1 31 10min-10-95 2 32 10min-10-95 3 33 10min-10-95 4 34 10min-10-95 5 35 10min-10-95 6 36 10min-10-95 7 37 10min-10-95 8 38 10min-10-95 9 39 10min-10-95 10 40 10min-10-95 11 41 10min-10-95 12 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- ' 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- ------ -- ---- --_ -- ---- -- --" ---- ----_ -- ---- -- ---- -- ---- ---- ---- -- **" ------ -- -- *" ---- -- -- -- "" ---- -- -- --- -- -- ------ ---- -- -- -- -- -- "" ----_ -- -- "" -- -------- ------ -- -------- ---- -- -- ---- -- -- ------ -- -------- -------- ------ -- ---- -- -- ------ -- ---- -- -- ------ ---- -- ---- "" FACT: D A T A REVIEW SUMMARY FORM Date: Data Analyst: FACT Study #: ' I n r / ' A r Matrix/Timepoints: Sample List / S is t& > __________________ ________ Set-up Analysis Date/Analyst: Instrument Q i/*? J>00\ Data Review Sign-OfT Analyst Review Name / Date:___ Technical Review . Name / Date: /Y l ? ' /o h JO I 1^'h Quality Assurance Review Name / Date:_____________ Data Entry:. inc, i t l n l n Ct OonmS mM eOnOts // JJui usutifuicu ai ti iuoinus:. - f j) , ? rv //2 A ^ Y /X L L ------- Acceptable L in r Raneer~\ LOQ: RA2: i ------------ L sju/i+s Extraction Blank: ^ J J z U * l. Matrix Blank: `/ l C Gl @ ^ d n f a p c ^ - ji / ? r 3 / sH t& ky J i iJ t* /o ^j>'Fpc Calibration Checks: - K M S/M SD:____________ AJjA-- ~ AO /tf ixrid . Data Status: m U FnbfiA ^^ K iyU ).ii lA i In /aq M b o f/- /&. A /r b ^ r , %-----------------------------------------( $ ) { / / / / / w / y y - Z / ^ Q /n ? /7 ^ a ^ Analyte: 'F p jT T S b f > & & F 7-- Acceptable Linear Range: LOQ: Q. C // ~> RA2: /7 . 0 * 9 ('s? Extracted Blank: Matrix Blank: ^Z ' ,FQ - Calibration Checks: M S/M SD : / ? A ^ ________________________ _____________ iiflVr, rinV U i e d p i pata Status: ______Vd lz- IAC c / / ^ 7 / /iT V i ^ /y T L ^ --------------------Q x /jliJ -h * m S - f a n f M /a /A a ~ &r>p* / / / r ^ jb 0 4 Analyte:: ^ U < T - 1 Calibration Checks: M S/M SD:________ Data Satus: Extracted Blank:_ Matrix Blank: ~v^ E * I ! UMM OOOOOOOO KIMMNWNUM WIUIVIUIUtLMUtWI O ui O ui OO utw O ui O ui OOOOOOQ vuiwuiuiuiui O ui O ui O ui O ui OO uiu O iu O iu O iu i . oM oM tfU oN oM Mo IVVW Mo Kq IoMoMoMoM oM oM c WMUlUIUtUIUII <S(O0tSiJ>IA Ou OaK) OMp Oo OmOogOVO -O O O QOOO gpOB OOOO gIUI O B OOO WMHQ OOOO <Bgg OOOO iUI^U ooooooe o jHOgo<(j o e o o 333333a a a . a a a s a a a a a f a a a s a a a a a a a a s a a a a a a a a a -- ii EEEEEEBBSSBEEEBEEEBEBEHEHESEaSMBBMEBHE^MBBfEBi EM>EEBS EEEEEE E E E E E E S S l IBUIUIWUMiigiUMUIUIUtVUlUlUIUIUIUIUIUIUIliUllBUIUIUIUtUlli M/iuiun/u>giuiviwi SiisigBilf^jfiiiigMjP.Mi000000000000 *>*< <1a ^ w i c i f i t i OH Ug IMOMB OH OM UU>B0 " ' ~ oeooeQ fiQ esssssll l l fff fSrSrS?S?iI HP P p tJ Wkl kitiaSi- * M PKI KKI HMI t MBi ) HH< mm `S-BJ B"jjBBBB HtlcOPMOH^OPg Bii iolaSoaBoi oi ao iI tIi< WiI iMU iHWMtWM WMt i Mu uMg mMuMi Bwbaa u h ui o - oo * i Sri _____ 1H V U Ox tOrPx BB **<w0 w0 w0 0w 0w I MMMMM MNBBBBB o SS BB fi rrssssg Beimi * sa 0# as fsloir >0000000000 hO kgBaO CHBHO UO* O O O O Off HI kMJ kHl HkJPkJk*l M B* UMMI HHM l i HNMR kHl kHl - jBEBB" H > M WMB SB sss a s 1?0 0 0 5 sssss 00* 55 s 'H M H >000 5SS55 HO OH OH OM OH ffrtflftfTffitii >lalala 1g g g 8888 i g g g 88 Ha B B iw^aa Jma naf ia a vvaiwjha Bm a B M *UW giBB 01 eta a 0000 0o o0o0o0o0i w0a0sc jgg g g g g g g g ggggggggggggggggggg, ggggg J N U M M N k l M U M M M N U P M w HMBk UI WB Uw Wu Wi pWCiI Wg BB Ww gWMBWpBgBMB W aWI B BB B B P P O kl agwkiggowoaHOBUBHOoaQk b w Q ` OBH I U B B g W kl 1H *B O B M O M U< P gU p . g B BB BB O B B U I W v w u g u w Ng gP Pw b ki * iggeBgwBoaUBggNH fi )BgwwMOkigggBgguBwgBl $$%$%$$$$SggggggSgKKggi gggggggggggggggS9gi ggg3 a gp oa aw gh g u p eguHBug*""***B U M H H t " g B g w ( - w p* o g g w p MW P O P W O P M P kBBMklWWklOBklOt ! l\ " l~c 1% MM P O " ilP H t R B w n s s ssglfsfgl ! g! P B kl e iU U k HOMO mw w O Vi m --r O H I N(1 n IO h hB N I''h'H <flilN rf)N II''55"22; H r4 0 4 14 r* S O H H H M H H r 'O >H4404Mr>0 nr. H 4 M n H n H O >4f4>atr4tff4<n <3c- i i 8 S S S S iiS 3 S S 2 S S sS H0 H Mn H r '40o4o<4'`l^f1 HHN4MHO ** 0otof4l NN0* nn l MH<i*n< fln *1 t Hr4S< A*l r1 * N'>H'!0r4O'444<r* *n4 rh<4- Hri>cH*nr<nHtinf4riN>4 - H-IO4 l0mNO 4HfiVhr>*r4*< thHfioonv 4 * m r- * 8<l f lrO mOfm1 < 4J Oi 4rB 4r ti rr t*4* 4O4M r' 0- t4' l*>nl*i 4no*afN4 ^0 i044r *t i "M0202 W5 2 Oi 2r2`N 2 2' M" S" ` p` tr-r*t*r.r ^ r> a ~rS O uo IT es-- <r- <s~ c* ; 3 ; ii 8 ti. ia Bsg: iS I 83 t.f.1** -1H a l|l 13881 8 8888 Ol Ot O* * A fitl 3 lllllllll Ho o4 Ho Ho Ho oH Ho Ho oH Ho aa,,Ha-,,-aaaSSSSS_: 8HS8 o o o o SSSSSj is". XX.X.X.SX.4aB. 858 O Oi O1 oQn s s a 3 aa sX.sX.3aX-mIBVl.iaBtS>S> aa 8"" mmhSBmhm nNHMNiuWHH H H M SIMM 2IHjlH* ". - fHlHMHI iHN HI 'i|||SS8 5 eSSo2 2 2 c jiggggggggggg I ioHNn4vi4h<OHr<n4 OOOOOOOOOOOOOOOO inininS'0o0'A>ov0'O4>or>r'r*ra r'r'r>h-r'r'<DM ooooooooooooooooooooooooo J S o o o g S o o S S o S ooooooinioiAinioo lS ig NS NNN N NN N NN S " inooooooiniii./i.in.otilnAO*KiiViin0t'nOi<n MNI 1o Ng M NNgNN bM No No tg Jo5ooJo o; or`o" DWO H n rt 4 o 3 Soup 020199: Quantified u d prtacad toy M M a 10/20/99 Soup 030199: QuAStlflod sad pr i aead toy MOI MoU1MoU<WoUKoIUto<MoUMI UoMtoUNI oUK<IoUMotMUo>MUoMI UoMI UoMIWoMUoIMUo<MUoMtUoMIUoMIUoM<oUM<oWUo>MoUMtoMNUoMMoMJ IoUMIoUMI UoMI WoMUoMI Uo)MUoMtUoMI WoMMoWMoUtMJoMWoNUoWMUoMI IoMwfll oooooooooooooooooooooooooooooooooooooooooooo 2? a P r p p Qx ,, P HT D o aaaaaaaaaaaasaasaaasaasaaaaaaasaaaaaaaaaasasss BeESBEEEBEBBBBBBBBBBB8BBBBBBB8BBBBBBBBEEBEgi U>U>U*UimVI/IV^VUtUIUIWVIU*V>V<tfUIVtiVUIUIUIVIVIUIVIU<U<WVM/>W<W>MWUtU>VV gsgggEsssIisslli t0- 0. M0M0' H0M 0> H0 H0H0M >0 -0H0M eh oM*eH oH I 4t I 4 I eH oM*uI oI I II wa MHHMHHHMMHMM oooooooooooo h lltlllllllll HoeUtMHtfM HW MM R KtIo tItoftI4o tIoMoc jMou ioMw oiMxowM M N M M Ul Ul Ul V* Ut wtIe Iu uWo Uuo eMw owMouM M M \nKi ei< ei t ei v )it e(>)e te >i e 'ie yt o i H JieWHM 'WHiH Xet Ss sSH8 3I ?S st lf lt S7 5| i. &7777,!.C . . E H1M M K N > ' IhT>hK Hi MM toM M MM MM NM MtMoMHI MHI M* a a a B S BBB - g SI Sl SlSiBnE g s 7777' ' SS? lOl Qn M Qn Pl fP * *<*< HI lH I# H^I "K - U>U>t rrBvlfi If IfS S S B B 77SSSSS HM Qr tKH H<M<H< HK H <HI ................ U>U>U>U>to arim i Sl 8!SI3!8ffaf5f7si5i . I7777J-C..E HT HN MW MH HW N M M ' hK hK iM w> t ot * oMt oM.MM,NM,M MwM MMI MM *W gasas--8 - -g B8 ' i l s SS ' SSSES BB 88 I W . be SQM Oi Ol lO MHH mM M ooooo H HwM H< He tototototo I'b b b b . ot oi lo loo M5M5H5M5* M5 ooooo H wH H wH wH tototototo :::pn hiih 3utoMUHMtototo QOQO QQ tototounutototo t) 2 S if il", t5 M i M f H r M l*4 i H "M O- B- M"X : m :s H !l S3 W MM HOMO 8 mt 1rs \ Ii sr <-i a. 4 J 4 4 4 I 4 J *4 4 4 4 > J 4 J J 4 r- U W W W W M M W U M W W M U M H MM W U W U M M M M U M W > g g ^ j O H * H totooto o OOHOWutaieoM* s > j H M e > a g g W H n a M o u a a a a o ^ g r a f > w g t f * g w u g i a uiHUiooviggaH<i'Ju<oou<>JwowMH*HHuv)ogoo - A s g & g m s m m m s s m m m m m m g g g g g g s| ~C> r-O ` OOOM OHHOOOOOOOOOOOOOOOOOOOOOHOOOOOOOOM I H IIIIIIIHI I I I I IM II i ft M H H I I MOI I H*tototototoOHI tot ot ot ot oOl I I H I I M t M ioaaauaMHgoaoa'iooaaaaoHtoaaaaaoaaMwaaa<JuaH 5 J /5 Soup030199: Qua&tlfld Mdprtatad bar oo 10/39/99 2 oup 0201t91QuAStlfladadprlatid toyMMIoo 10/2(/tt Quantify Calibration Mpert ton 145: Rat torn. Day 1*4 dilation*. Btt 10/19/9 Compound 3 name: Surr Response Factor: 3154.38 Response type: External Std, Area Curve type: RF 3.77e3-i x * * XKKXX OOP 030199: Quaatifiad and printad by MMi on 10/35/99 Method Report Nathod file: Last modified: Ccnpound: Printed: C: \JUSSLYKX\soup020199 . p r o \ M e thDi\102599b.mdb Tua OCC 26 09:1131 1999 FFOS T u a OCC 2 6 1 0 1 4 t : 1 4 1 9 9 9 Coeqpound Man e : Internal Ret.: Quantify Traca: Cone, of Standard*: Osar RP Valua: User Peak Factor: Integrate Window Factor: Chromatogram mass window Ratantioa Time (mins); Ralativa Ratantioa Tin RT Reference: Tina Window (mins): Paak Salactioo; pros (R enal TIC Cone. A 1.000000. Disabled 1.000000 2 .0 0 0 l.OOOODa 7.490, Bnablad 0.000. Oisablad (one] 0.312 Rasponsa Type: Rasponsa: Folynonial Typo: Point of Origin: Fit Weighting: Axis Transformation: 1 iima r bcluda 1/X Ron* Units: Peak*to-peak aaplituda: 76 Snoothing: Window size (scans): Number of naooths: Smoothing nathod: Join vallay threshold: Reduce paak tailing: Raisa baseline maximum: Enabled 2 1 30.00 200.00 S.00 Draw vertical threshold: Detect shoulders: Shoulder threshold: 90.00 Disabled 30.00 Ralativa height: Absolute height: Relative area: Absolute area: 1.S0. Disabled 0.00. Disabled 2.00. Disabled 0.00, Disabled -- ^4^5 Method Report Method file: L M t modified: Compound : Printed: C : \KRSSLYlCC\aoup020199.pro\MethDB\102S99b.mdb Tue Oct 26 09:11:11 1999 2 : PfOSA Tue Oct 26 10:11:14 1999 Compound Mame: Znternel Ref.: Ouentify Trace: Cone, of Standards: Oser Rf Value: Oeer Peak factor: integrate Window factor: Chromatogram mass window Retention Time (Bine): Relative Retention Time: RT Reference: Time Window (nins) : Peek Selection: Response Type: Response : Polynomial Type: Point of Origin: Pit Weighting: Axis Transformation: pfosa (Hone] TIC Cone. B 1.000000. Dieabled 1.000000 2.000 1 .00000a 7.9(0. Enabled 0.000, Disabled (Monel 0.400 Meareat 1 Areas linear Exclude 1/z None Units: peak-to-peak eaplitude: 7( Smoothing : Window else (scene): Number of mnootha: Smoothing method: Enabled 2 1 Join valley threshold: Reduce peak tailing: Raiae baseline atximm: 30.00 200.00 5.00 Drew vertical threshold: Detect shoulders : Shoulder threshold: 90.00 Disabled 30.00 Relative height: Absolute height: Relative aree: Absolute eree: 1.50. Disabled 0.00, Disabled 2.00, Disebled 0.00, Disabled Method Report Hattiod Ell: modified: Ceepaund; Printed: Ct^ttSSL^na\*op0201" P^oV,, thD X10J5,*b *dl, Tue Oct 26 09:11:31 1999 ]: Surr Tue Oet 26 104:14 19 Compound Nu n : Internal M i . i Quantify Trace: Cone- of Standards: User W Valua; Osar Peak Factor: integrate Window Factor: Chromatogram ease window: Retention Tina (nine): Relative Racantion Tine: RT Reference: Tina Window (nine) : Peak Selection: Response Type; Response: Polynanial Type: Point of Origin: Fit Weighting: Axis Transformation: Surr {Monel TIC Fixed 1.000000, Disabled 1.000000 2.000 l.OOOODa 7.245, enabled 0.000. Disabled (Mona) 0.101 Nearest external Areas linear exclude 1/X Mona Units: Peak-to-peak amplitude: <5 Smoothing: Window site (scans): . Humber of snnnthe: Smoothing method: Join valley threshold: Reduce peak tailing: Raise baseline maximum: Draw vertical threshold: Detect shoulders: Shoulder threshold: Relative height: Absolute height: Relative area: Absolute area: enabled 2 1 30.00 200.00 5.00 90.00 Disabled 30.00 * 1.50. Disabled 0.00. Disabled 2.00. Disabled 0.00, Disabled /& Quattro II, #6414E SOUP 020199: FACT Equipment Log 99092 PAGE 1/1 DATE: 10-25-99 ANALYSTrmmmh C T im v NUMBER: TOX145 MATRIX: Rat sera DESCRIPTION: Dilutions FACT Method: ETS-8-5.1 Injection volume: 10 uL Cycle time:,lQmjp: Electrode: --------- Mobile Phase: iKY> n mM NH4CH3C02 (B) MeQH------------------- TN-A- or stndrd number (A) 99085-11-3------------- Prepared (date/by): Expires: 10/21/99 tximh_______ <X) 04/00______________ (B) TN-A-299?------------- (B) \QI\(ff99 sah (B)_2fllQ--------------------- Store at room temp? @ or N O th e r-------- Guard column: None___________ _______ Part number: na_________ Lot number:_na-------- Analytical column: Keystone Betasil_________________ Size: 2 x 50 mm_______________ . Type:_18----------Part nnmher: 055-701-2_________ Lot number: P9gH Sphere size: 5 um______ Serial number:0591804Z Analytical parameters: Drying gas fL/hrl: 350 ESI nebulizing gas (L/hr)_12___ Sheath gas (L/hr)_0 LC Flow rate: 300 uL/min. Back pressure: $5 bsr_ HPLC solvent gradient: 10min-10-95 Time (min.! n o.oo_________ 2) _L2Q______ 3) i 5 f i _______ 4) JL50_______ 51 8.00_________ %B 100 m 0_ -210 210. m il Tuning Method Report Method: C :\MASSLYNX\SOUP-RATS.PR0\ACQUDB\PP0S3 Printed: Mon Oct 25 i6:37:32 X999 Page 1 MS SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. MS Set Rdbk 1.60 60 5 0.2 150 250 1.60 -60 -6 151 250 Pressures Analyser Vacuum Gas Cell Rdbk 5.9e-5 4.le-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set Rdbk 14.0 14.0 0.9 0.0 4 650 3 Set Rdbk 14.0 14.0 60 2.0 0.0 40 0 650 42 38 44 B . .. B U A ftltJM l B A W M * Matted: Cj\MRSSWME\S0UF-lttTS.P*O\*C0OTM\10liI-WO9-Ote-P?OA-Il teat Modified: Fri Oct 15 ll:3Si03 1959 Printed: Moo Oct 35 18:38*34 1999 Solvent Dalay ( Bias > : 0.00 Function : 1 M m of 1 Mesa Fair ( > Intar Channel Dalay <[ Sacs ) : Span ( Daltons ) i Start Ti*e ( Mina ) : Bnd Tina ( Mina ) : Repeats t Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Scea) Coll Energy (eV) Coiia ( V ) 1 413.00 1C9.00 0.30 30 15 Function : 2 M M of 1 Xaaa Fair ( t - ) Inter Channel Delay 1[ Sacs ) : Span ( Daltons ) : Start Tina ( Mina ) : End Tina ( Mina ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Saca) Coll Energy (aV) Cona ( V ) 1 499.00 99.00 0.30 . 45 CO Function : 1 M M of 1 Mean Fair ( m - ) Inter Channel Delay 1( Secs ) : Span ( Daltons ) > Start Tiaa ( Mina ) : Snd Tina ( Mias ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Sacs) Coll Energy (aV) Cona ( V ) 1 498.00 78.00 0.30 45 CO Function : 4 M M of 1 Mass Fair | I - ) Inter Channel Delay <( Secs ) : Span ( Daltons ) : Start Tiaa ( Mins ) ; End Tiaa ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Sacs) Coll Energy taV) Cona ( V ) 1 427.00 80.00 0.30 40 CO Mathod Report Method rile: Last Modified: Printed: cs \aaalyruc\aoup-rata.pro\acqudb\lQmin-10-9S Honday# October 25/ 1999 16*29x58 Monday/ October 25/ 1999 16i34t46 HP1100 LC Pump Znltiel Condltione Solvents A% B% C% D% 90.0 10.0 0.0 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) -3 10.0 0 400 30.0 30.0 HP1100 LC Pump Oradient Timetable gradient Timetable contains 5 entries which Time A% B% C% D% Flow 0.00 90.0 10.0 0.0 0 . 0 0.300 1.00 90.0 10.0 0.0 0 . 0 0.300 5.50 5.0 95.0 0.0 0 . 0 0.300 7.50 5.0 95.0 0.0 0 . 0 0.300 8.00 90.0 10.0 0.0 0 . 0 0.300 HP1100 LC Pump external Bvant Timetable The Timetable contains 3 entries which are : Time Initial 0.00 0.10 Column Switch Contactl Off Off Off On Off Off Contact2 Off On Off Contact3 Off Off Off Contact4 Off On Off HP1100 Autoeampler Initial Conditions Draw Speed Eject Speed (pl/min) Draw Position (mm) Stop Time (mins) Injection Volume (ul) Vial Number 200.0 200 0.00 9.00 10.0 9 Page x/o-XS^9 Pressure 400 400 400 400 400 Masslynx - Sam ple List Sample Ust: C:\MASSLYNX\soup-rats.pro\SampleDB\102599b.SPL Printed: Mon Oct 25 16:32:57 1999 Page 1 P age Position: (1,1) File Name Pile Text MS File 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 102599039 MeOH Blank 102599040 MeOH Blank 102599041 TOX145-RBS10199-H 20 Blk-12, SEE 102599042 TOX145-RBS10199-Serum Blk-12, SEE 102599043 TOX145-RTS10199-Serum Blk-12, SEE 102599044 TOX145-RBS10199-5ppb-12, SEE 102599045 TOX145-RBS10199-10ppb-12, SEE 102599046 TOX145-RBS10199-25ppb-12, SEE 102599047 TOX145-RBS10199-50ppb-12, SEE 102599048 TOX145-RBS10199-100ppb-12, SEE 102599049 TOX145-RBS101'99-250ppb-12, SEE 102599050 TOX145-RBS10199-500ppb-12, SEE 102599051 TOX145-RBS10199-750ppb-12, SEE 102599052 TOX145-RBS10199-1000ppb-12, SEE 102599053 MeOH Blank 102599054 TOX145-RTS-9R03245M, Dayl, 5mg/kg, D50-ext10/19/99 102599055 TOX145-RTS-9R03246M, Dayl, 5mg/kg, D50-ext10/19/99 102599056 TOX145-RTS-9R03247M, D ayl, 5mg/kg, D50-ext10/19/99 102599057 TOX145-RTS-9R03248M, D ayl, 5mg/kg, D50-ext10/19/99 102599058 TOX145-RTS-9R03249M, Dayl,5m g/kg, D50-ext10/19/99 102599059 TOX145-RBS10199-250ppb-CCV-11-1, SEE 102599060 TOX145-RBS10199-250ppb-12, SEE 102599061 MeOH Blank 102599062 TOX145-RTS-9R03250M, Day4,5mg/kg, D50-ext10/19/99 102599063 TOX145-RTS-9R03251M, Day4, 5mg/kg, D50-ext10/19/99 102599064 TOX145-RTS-9R03252M, Day4, 5mg/kg, D50-ext10/19/99 102599065 TOX145-RTS-9R03254-1M, D ay4,5mg/kg, D 50-10/19/99 102599066 TOX145-RTS-9R03254-2M, D ay4,5mg/kg, D 50-10/19/99 102599067 TOX 145-RBS10199-250ppb-CCV-11-2, SEE 102599068 TOX145-RBS10199-250ppb-12, SEE 102599069 TOX145-RBS10199-250ppb-CCV-11-3, SEE 102599070 TOX145-RBS10199-250ppb-CCV-11-4, SEE 102599071 MeOH Blank 102599072 TOX145-RBS10199-H 20 Blk-12, SEE 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 1OMIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10M IN -PFO S-PO A A -PFO SA -IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 1OMIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 35 102599073 TOX145-RBS10199-Serum Blk-12, SEE 36 102599074 TOX145-RTS10199-Serum Blk-12, SEE 37 102599075 TOX145-RBS10199-5ppb-12, SEE 38 102599076 TOX145-RBS10199-10ppb-12, SEE 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 39 102599077 TOX145-RBS10199-25ppb-12, SEE 40 102599078 TOX145-RBS10199-50ppb-12, SEE 41 102599079 TOX145-RBS10199-100ppb-12, SEE 42 102599080 TOX145-RBS10199-250ppb-12, SEE 43 102599081 TOX145-RBS10199-500ppb-12, SEE 44 102599082 TOX145-RBS10199-750ppb-12, SEE 45 102599083 TOX145-RBS10199-1000ppb-12, SEE 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS M asslynx - Sam ple List Sample st: C:\MASSLYNX\soup-rats.pro\SampleDB\102599b.SPL Printed: Mon Oct 25 16:32:57 1999 Inlet File Bottle Inject Volume Sam ple Type C one A C oncB C one C 1 10min-10-95 91 2 10min-10-95 91 3 10min-10-95 21 4 10min-10-95 22 5 10min-10-95 23 6 10min-10-95 24 7 10min-10-95 25 8 10min-10-95 26 9 10min-10-95 27 10 10min-10-95 28 11 10min-10-95 29 12 IOmin-10-95 30 13 10min-10-95 31 14 10min-10-95 32 15 10min-10-95 92 16 10min-10-95 33 17 10min-10-95 34 18 10min-10-95 35 19 10min-10-95 36 20 10min-10-95 37 21 10min-10-95 43 22 10min-10-95 29 23 10min-10-95 92 24 10min-10-95 38 25 10min-10-95 39 26 10mir>-10-95 40 27 10min-10-95 41 28 10min-10-95 42 29 10min-10-95 44 30 10min-10-95 29 31 10min-10-95 45 32 10min-10-95 46 33 10min-10-95 93 34 10min-10-95 21 35 10min-10-95 22 36 10min-10-95 23 37 10min-10-95 24 38 10min-1O-95 25 39 10min-10-95 26 40 10min-10-95 27 41 10min-10-95 28 42 10min-10-95 29 43 10min-10-95 30 44 10min-10-95 31 45 10min-10-95 32 10 -- 10 -- 10 -- 10 -- 10 -- 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 QC 10 QC 10 -- 10 -- 10 -- 10 -- 10 -- . 10 -- 10 QC 10 QC 10 QC 10 QC 10 -- 10 -- 10 -- 10 -- 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard -- -- -- -- -- 4.93 9.76 24.8 49.3 97.6 248 493 735 976 -- -- -- -- -- -- 248 248 -- -- -- -- -- -- 248 248 248 248 -- -- -- -- 4.93 9.76 24.8 49.3 97.6 248 493 735 976 -- -- -- -- 4.93 9.77 24.8 49.3 97.7 248 493 736 977 -- -- -- -- -- -- 248 248 -- -- -- -- -- -- 248 248 248 248 -- -- -- -- 4.93 9.77 24.8 49.3 97.7 248 493 736 977 -- *** _ -- -- -- _ -- -- --* -- _ -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- --- . -- -- -- -- -- -- Page 2 P age Position: (2,1) FACT: DATA REVIEW SUMMARY FORM Date: DataAnalyst: FACT Study*: ' i v t t / S ' . Matnx/Timepoints: + //, * r j (fa Sam ple LixL / A ^ ^ h ------------------ ---------- Set-upAnalysia Date/Analyst: /erT - j Ct? ) \ Instrument Analyte:. 1 > 0 & 0 - Acceptabte Linear Range: "^ff-Q.____ O - TOO j f . f l t o k z ) FrtraetinnBlank: ^ ^h C D O .__ Ra2; f l Matrix Blank . /) Q -- CalibrationChecks: _______ ____________ _______ MS/MSD:________ K )o \ JyiiCaA loiHv ?DA/^------------- Data Status: 0 ) Q ) ___________ E o W t A Ut Analyte:. m i Acceptable Linear Range: LOO: ~~ ~ R A2: '' CalibrationChecks: MS/MSD: DataStatus: (M - Analyte:. ExtractedBlank Matrix Blank CalibrationChecks: MS/MSD:_____ DataSatus:____ ExtractedBlank. Matrix Blank Data Review Sign-OfT Technical Review Name/ Date QualityAssuranceReview Name/ Date:_________ DataEntry: _ eJ w LAC l o l w h l . Comments/ Justifications: {]) t///>////// * / A ^ // j /vb n r f c j^ c ^ jnoeL A-M iyn h i t f /2r? j u a A < JA f 0^ ^ = . V zkA - m /tA ? / J d /A ,_______________ .-- :Al-Zf?? 0 #J0 ,,Y>(r>*s . rU / (/? /* /la n o /fi/rfi/7/r> f i f r/2/g- /K * Q uj//j 'SbA - * f t y j b i W S t i L _______ tir a t i f 0 b p u f A ir - r ^ ^ . Q w s i f 'n C j f X J / p v f (0 ) ^/-r<SvSgS~^~g s ^ M ^ L - l ------------------J a . =*s/>o*isC. ) fj< ^ V U ^ ( jv & j- r * w r /o * J ( S ^ ^ i k j r ' ) s J S > ^ u a l 7 \ . A l o d t - # ? s <a 5 y r i/J Ao<Ni-re-)t- S / & o - { / 3 ^ r ~ S ~ . j / k ^ q a t Awa-MT i s gggsssssgs IsassIlllasiaaaaaaaaaaaaaaaaaaaaaaaaaasaaaaaasasajilaliliSaal ugggggggSoSFSSSgggoggSgggggg-SfiSSSSggSSSgSggggSggggggSSSSS!!; l ' ~ g S f S S R <:; 0' E e; g 0'S S S 2 g S S g 3 c: 2 0' S ? g ; 1 Dvy 070799: q u M t i U U d and p r u t U d by U 0 / 2 I / 9 9 "SfssisSISsiliissSajSSsssssjSiISSsssSsissSsSISISsIs IS: SSjeSSSSSSS ---= 255 gg^sssgggg ---=ss =25 ggggg 22222 33333 m\ :gggg 2522 3 3^ 3^ 3^3 ni ggggg 33333 3!3l3!33 S 2g g2 g2 :23 3 3i33 31.' gg 22 33 s liiii lilil mil, S* MR?, , i' . v | | l l l assB . . . . . . . . . . B ............ 3 - - " i i " 2 Smij tllth lll^"-i aai| r " . l i i i s i i i i y i y i j i i t iyi i f f l i ! ! ! ! llliiliiiiiilliiiliSiiiiiiiiiiiiiiillilBlliiBilBlIlBigi 2=22222 ' " M r ' - J" t" ' " " 2 2 2 2 = 2 2 2 2 2 S 3 3 2 = S S 2 S S S 3 3 2 ? ;s S S S ;;SS2223SSKSS G> ~7 ~T^ SSS >r > V2P- ss II i a a a a lll SSSSSPPSSS asssssg i \ s s Ss =| | a aaaaaa aaaaaa asa S CSS2S3 SSSSPE SSS 3 H i m SPSS i laaaaaaall SSSSSSSSSP " -asggssg I 3 m m 1511 a s S 5 5 | | S | | fi s s s s s s s s s s I SSPSSSSSSo " -"sags s s s s s s s s s s s s s S5S I~! (J fj r- r-'r-"r~ r- r- r- r- t- g g SS i i ii SsSSSSSSss r-r-r*r*i-r'f'*f~rr- sppsssssss "" n u n 11111 11111 UHI Siili ,, l i l i ! 111! 11111 111 .,,,,i lililUnti IflfiIfIJJii il IU I1 Davay 07079: quantitatad and printed by aahlO/29/99 ""SPSasSSSSSSSSiSSSSRSSSiSaSSSSSSSSSSSSSSSSSSasSXSSS I |gg??S''`2 S 2 r-222gS3SS;50 g::22''773S277"|'f?22",',|SE2g22:25SSS: S77 1 1 1 *7 7 7 1 S2222222222222222222222222222222222222222222222222222222222 3ggg32g223SgSSEgSSSS52g322SS:SgS22S;S3ggS22gggSE2g22S2SSSS::SSS SHHCHJH^H(joO^H-HHO^^cJoOHr-do^OOOH^Hr40H-HHO^HOH--HHHHHO is=|l|" B s i l l i I l l " 2 RI s l s s 3 slilililll crcr* "o- S=s s s ; ? l l s l 3 s i l l s i i ? ! ! 2 ? i s s s i i g i i l s l s l ^ ' ' O ' * ' * * * ' * * ' * ' * * ' * ' * ' * * ' ' * ' * ' * ' 0 '* o 5 1 gggggggggg gggggggggg " 5 *-* 2 S5SSS sssss III SSS53 m il -sssS ss gg !!! SSS^ ss 22 ss -~ I I W m n m s i " 35 c <i c I I , 1 1 I I i ! , I i=,333 l i i l 1 lili1 illl Dtvay 070799: quantitatad and printad by hlO/29/99 - ^ ^ ^ " - S;;3:j:;sst:5 2 g s S ja 5 S S K 5 S g s 5 ! S S S S E 5 S S S g 3 = 2 E 5 ; S S S 3 S S S E S S />~L$-'e? c? - i s Dtvay 07079: quantitat*d and p n a U d by hlO/28/99 Quantify CAlibtktieo Raport Tox 115: Rit tart and L i w , Day 1 1 1 9* 2 Davay 070799: quantitatad and printad by aahlO/29/99 Quantify Calibration Alport Tox 143: JUt Sara and Lavas, Day 1 & 4 Davwy 070799: quantatatad aad prlntad toy Mhl0/2t/99 Method Report Method file: U s t modified: Compound: Printed: C:\HASSLYNX\Davey070799.PRO\MethDBU02799b.mdb Thu Oct 28 08:57:32 1999 1: PQAA {func 1) Thu Oct 28 12:11:03 1999 Compound Naae: Internal Ref.: Quantify Trace: Cone, of Standards: User RF Value: User Peak Factor: Integrate Wind Factor: Chrcmetograa bass winde: POAA (func 1) (None] TIC Cone. A 1.000000, Disabled 1.000000 2 .0 0 0 l.OOOODa Retention Tine (Bins): Relative Retention Time: RT Reference: Time Window (mins): Peak Selection: 8.842, Enabled 0.000, Disabled (None) 0.414 Nearest Response Type: Response: Esternal Areas Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Linear Exclude 1/* None Units: Peak-to-peak amplitude: Smoothing: Window size (scans): Number of smooths: Smoothing method: Join valley threshold: Reduce peak tailing: Raise baseline maximum: Draw vertical threshold: Detect shoulders: Shoulder threshold: Relative height: Absolute height: Relative area: Absolute area: 492 Disabled 1 1 Savitzky Golay S.00 50.00 10.00 25.00 Disabled 5.00 1.50, Disabled 0.00, Disabled 2.00, Enabled 0.00, Disabled Method Report Hathod ill.: Last modifiad: Compound: Printed: C:\MASSLm\Dw.y070799.PKO\M.thDB\102799b.Bdb Thu Oct 28 08:57:32 1989 2: 980 (func 2) Thu Oct 28 12:11:03 1999 Coapound Na m : Intarnal Aaf.: Quantify Traca: Cone, of Standards: Usar RF Valua: Usar Paak Factor: Intagrata Window Factor: Chrcaatogram oass winder: 980 (func 2) (Nona) TIC Cooc. A 1.000000, Disablad 1.000000 2.000 l.OOOODa Ratantion Tiaa (mins): Ralativa Ratantion Tioa: RT Rafaranca: Tiaa Window (ains): Paak Salaction: Rasponsa Typa: Rasponsa: 7.620, Enablad 0.000, Disablad (Nona) 0.359 Naarast Extamal ' Arams ' Polynomial Typa: Point of Origin: Fit Waighting: Axis Transformation: Liaaar Sxcluda 1/X Nona Units: Paak-to-paak aapiituda: 4 Smoothing: Window siza (scans): Nunbar of saooths: Smoothing aathod: Disablad 1 1 Savitzky Golay Join valiay thrashold: Raduca paak tailing: Raisa basalina aaxiaua: 5.00 50.00 10.00 . Draw vartical thrashold: Datact shouldars: Shouldar thrashold: 25.00 Disablad 5.00 Ralativa haight: Absoluta haight: Ralativa araa: Absoluta araa: 1.S0, Disablad 0.00, Disablad 2.00, Enablad 0.00, Disablad Method Raport Last modified: Compound: Printed: C:\MASSLYNX\Davey070799.PRO\KethDB\102799b.mdb Thu Oct 28 08:57:32 1999 3: surr (fune 3) Thu Oct 28 12:41:03 1999 Compound Na b : Internal Af.: Quantify Trac: Cone, of Standards: Usar RF Valu: Usr Peak Factor: Integrate Window Factor: Chromatogram mass window: suer (fune 3) (Non] TIC Fixd 1.000000, Disabid 1.000000 2 .0 0 0 1.0000D Rtntion Tim tains) : Relative Retention Tim: RT Rafarane: Tina Window (Bins): Peak Selection: 6.B20, Enabled 0.000, Disabled (Non) 0.265 Nearest Rspons Typ: Rspons: External Aru Polynomial Typ: Point of Origin: Fit Weighting: Axis Transformation: Linar Rxclud 1/* Hon Units: Peak-to-peak amplitud: -- Smoothing: Window siz (scans): Number of ssooths: Smoothing mathod: Join vally thrashold: Reduc pak tailing: Rais baslina maxim: Draw vertical thrashold: Datact shouldars: Shoulder thrashold: Relativa haight: Absolut haight: Absolut area: 629 Disabled 1 1 Savitzky Golay 5.00 50.00 10.00 25.00 Disabled 5.00 1.50, Disabled 0.00, Disabled 2.00, Enabled 0.00, Disabled Pag 3 DAVEY 070799: FACT Equipment Log 99077 Q uattro Ultima: #9261QB PAGE DATE: 10/27/99 ANALYST:mmh STUDY NUMBER: Toxl45: Matrix: Rat Sera& Liver DESCRIPTION: PQAA& 980 FACT Method.ETS 8-5.1 & 8-7.0 Injection volume- 5 n l. Cycle time: 10 min. EleUiude. Z-Spray. Mobile Phase: l \ X>0 mM NH4CH3CQ2 (B )M eO H __ TN-A- or stndrd number (A) 99085-11-3_______ (B1 tn-a-2945 Prepared (date/by): fAl 10/23/99 sah_______ fBl 10/23/99 sah Expires: (A1 04/00______________ (B)_04/00_____ Store at room temp? @ or N Other Guard column: None_____________ _____ Part number: na________ Lot number: nn Analytical column: Keystone B e t a s i l ___________ ______________________ _______ Size: 2 x 50 mm_______________ _ Type:jCI8___________ Sphere size:J m n ---------Part nnmtvi- 055-701-2_________ Lot number: P9E11____ Serial number: 0591825Z Analytical parameters: Drying gas fL/hrl: 487 ESI nebulizing gas (L/hr)_10___ Sheath gas (L/hr)J)_ LC Flow rate: 300 uL/min. Back pressure: 82 bar HPLC solvent gradient: 10min-10-95 T11im0.e00(m__i_n_.l_____ 21 1.00________ 31 5.50________ 4 7,50_________ 51 8.00_________ %B 10.0 10.0 210 95.0 1M Tuning Method Report Method C:\MASSLXNX\DAVEY BACKUP AUG99\DAVEY-RATS.PRO\ACQUDB\PFOS-4 Page 1 Printed: Wed Oct 27 14:31:21 1999 SOURCE ( ESP- ) Capillary(kV) Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp. Set Rdbk 3.15 10 0.0 0.0 0.0 150 250 -3.07 -11 148 249 Pressures Analyser Vacuum Gas Cell Rribk OFF 4.3e 3 Analyser LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas Flows Cone Gas Desolvation Set Rdbk 14.5 14.5 1.0 -2 2 1 12.0 12.0 1.0 650 -3 2 0 -646 Rdbk 57.8 484.8 lcnnu>9 M ethod Kapert lotted: C :\jsiinnc\n*vEf0707.p*o\*counB\icini-io**-**0"15 L u t Modified: 1 M Oct 27 14:10:01 1999 rmted: Wed Oct 27 14:32:05 1999 Solvent Delay { aina ) : 0.00 rweticn : 1 M M of 1 IKsa Pair < ESP- ) Inter Channel Delay ( Secs > : Span ( Daltons ) : Start Tine { Mins ) : End tiae ( Kins ) : 0.03 0.00 0.00 10.00 R*P**tChinnel Parent Daughter Dwell (Secs) Coll Energy (eV) Cone ( V ) 1 413.00 169.00 0.30 30 15 rtneU.cn : 2 M M of 1 Maas Pair ( ESP- > Inter Channel Delay ( Secs ) : Span ( Daltons ) : Start Tiae ( Kins ) : End Tiae ( Mins ) : Repeats : Channel Parent Daughter 00.. 0003 0.00 10.00 1 Dwell . (Secs) Coll Energy (eV) Cone ( V ) 1 980.00 70.00 0.30 60 60 funoUw : 3 M M of 1 Maas Pair ( ESP- ) Inter Channel Delay ( Sacs ) : Span ( Daltons ) : Start Tiae ( Kins ) : End Tiae ( Mins ) : Repeats : Channel Parent Daughter 0.03 00 ..00 00 10.00 1 Dwell (Sees) Coll Energy (eV) Cone ( V ) 427.00 00.00 0.30 40 60 /Zr2> 7 - 9 ^ 9* 1 Method Report Method File: Last Modified: Printed : Page 1 C :\MASSLYNX\DAVEY070799.PRO\ACQUDB\10min Wednesday, October 27, 1999 14:25:05 Wednesday, October 27, 1999 14:25:31 HP1100 LC Pump Initial Conditions Solvents A% B% C% D% Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 90.0 10.0 0.0 0.0 0.300 10.0 0 400 30.0 30.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 5 entries which are ime 0.00 1.00 5.50 7.50 8.00 A% 90.0 90.0 5.0 5.0 90.0 B% 10.0 10.0 95.0 95.0 10.0 C% 0.0 0.0 0.0 0.0 0.0 D% 0.0 0.0 0 .0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 HP1100 LC Pump External Event Timetable The Timetable contains 3 entries which are : Time Initial 0.00 0.10 Column Switch Contactl Off Off Off On Off Off Contact2 Off On Off Contact3 Off Off Off Contact4 Off On Off HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (ul/min) Draw Position (mm) Stop Time (mins) Injection Volume(ul) Vial Number 200.0 200 0.00 9.00 10.0 12 M asslynx - Sam ple List Sam ple List: C:\MASSLYNX\Davey070799.PRO\SampleDB\102799b.SPL Printed: W ed Oct 27 14:34:05 1999 /C r< J iL<?7 Page 1 P age Position: (1,1) File Name File Text 1 102799013 MeOH Blank 2 102799014 MeOH Blank 3 102799015 TOX145-RBS10229-H2O Blk-1, RWW 4 102799016 TOX145-RBS10229-Serum Blk-1, RWW 5 102799017 TOX145-RBS10229-1ppb-1, RWW 6 102799018 TOX145-RBS10229-5ppb-1, RWW 7 102799019 TOX145-RBS10229-10ppb-1, RWW 8 102799020 TOX145-RBS10229-25ppb-1, RWW 9 102799021 TOX145-RBS10229-50ppt>-1, RWW 10 102799022 TOX145-RBS10229-100ppb-1, RWW 11 102799023 TOX145-RBS10229-250ppb-1, RWW 12 102799024 TOX145-RBS10229-500ppb-1, RWW 13 102799025 TOX145-RBS10229-750ppb-1, RWW 14 102799026 TOX145-RBS10229-1000ppb-1, RWW 15 102799027 MeOH Blank 16 102799028 TOX145-RTS-9R03230M, Day1, control,-ext10/19/99 17 102799029 TOX145-RTS-9R03231M, Day1, control,-ext10/19/99 18 102799030 TOX145-RTS-9R03232M, Day1, control,-ext10/19/99 19 102799031 TOX145-RTS-9R03233M, Day1, control.-ext10/t9/99 20 102799032 TOX145-RTS-9R03234M, Day1, control,-ext10/19/99 21 102799033 TOX145-RBS10229-250ppb-1, RWW 22 102799034 MeOH Blank 23 102799035 TOX145-RTS-9R03235M, Day4,control,-ext10/19/99 24 102799036 TOX145-RTS-9R03236M, Day4, control,-ext10/19/99 25 102799037 TOX145-RTS-9R03237M, Day4, control,-ext10/19/99 26 102799038 TOX145-RTS-9R03238M, Day4, control,-ext10/19/99 27 102799039 TOX145-RTS-9R03239M, Day4, control,-ext10/19/99 28 102799040 TOX145-RBS10229-250ppt>-1, RWW 29 102799041 MeOH Blank 30 102799042 TOX145-RTS-9R03245M, Day1, 5mg/kg, D50-ext10/19/99 31 102799043 TOX145-RTS-9R03246M, Day 1, 5mg/kg, D50-ext10/19/99 32 102799044 TOX145-RTS-9R03247M, Day1, 5mg/kg, D50-ext10/19/99 33 102799045 TOX145-RTS-9R03248M, Day1, 5mg/kg, D50-ext10/19/99 34 102799046 TOX145-RTS-9R03249M, Day1, 5mg/kg, D50-ext10/19/99 35 102799047 TOX145-RBS10229-250ppb-1, RWW 36 102799048 MeOH Blank 37 102799049 TOX145-RTS-9R03250M. Day4, 5mg/kg, ext10/19/99 38 102799050 TOX145-RTS-9R03251M, Day4, 5mg/kg, ext10/19/99 39 102799051 TOX145-RTS-9R03252M, Day4, 5mg/kg, ext10/19/99 40 102799052 TOX145-RTS-9R03254-1M, Day4, 5mg/kg, ext 10/19/99 41 102799053 TOX145-RTS-9R03254-2M, Day4, 5mg/kg, ext 10/19/99 42 102799054 TOX145-RBS10229-250ppb-1, RWW 43 102799055 MeOH Blank 44 102799056 TOX145-RTL-9R03247-M, Day1, 5mg/kg, ext 10/13/99 45 102799057 TOX145-RTL-9R03253-M, Day4, 5mg/kg, ext 10/13/99 46 102799058 TOX145-RBS10229-250ppb-1, RWW 47 102799059 MeOH Blank 48 102799060 TOX145-RBS10229-H2O Blk-1, RWW 49 102799061 TOX145-RBS10229-Serum Blk-1, RWW 50 102799062 TOX145-RBS10229-1ppt>-1, RWW 51 102799063 TOX145-RBS10229-5ppb-1, RWW 52 102799064 TOX145-RBS10229-10ppb-1, RWW 53 102799065 TOX145-RBS10229-25ppb-1, RWW 54 102799066 TOX145-RBS10229-50ppb-1, RWW 55 102799067 TOX145-RBS10229-100ppb-1, RWW 56 102799068 TOX145-RBS10229-250ppb-1. RWW 57 102799069 TOX145-RBS10229-500ppb-1, RWW 58 102799070 TOX145-RBS10229-750ppb-1. RWW M asslynx - Sam ple List j Sam ple Ust: C:\MASSLYNX\Davey070799.PRO\SampleDB\102799b.SPL Printed: W ed Oct 27 14:34:05 1999 / r< J Page 2 P ag e Position: (2, 1) MS File Inlet File Bottle Inject Volume Sam ple Type C one A 1 10MI N-POAA-980-IS 10min-10-95f 91 2 10MIN-POAA-980-IS 10min-10-95f 91 3 10MIN-POAA-980-IS 10min-10-95f 1 4 10MIN-POAA-980-IS 10min-10-95f 2 5 10MI N-POAA-980-1S 10min-10-95f 3 6 10MI N-POAA-980-1S 10min-10-95f 3 7 10MI N-POAA-980-IS 10min-10-95f 4 8 10MI N-POAA-980-IS 10min-10-95f 5 9 10MIN-POAA-980-IS 10min-10-95f 6 10 10MIN-POAA-980-IS 10min-10-95f 7 11 10MIN-POAA-9804S 10min-10-95f 8 12 10MIN-POAA-980-IS 10min-10-95f 9 13 10MIN-POAA-9804S 10min-10-95f 10 14 10MIN-POAA-980-IS 10min-10-95f 11 15 10MI N-POAA-980-IS 10min-10-95f 92 16 10MI N-POAA-980-IS 10min-10-95f 12 17 10MIN-POAA-980-IS 10min-10-95f 13 18 10MIN-POAA-9804 S 10min-10-95f 14 19 10MI N-POAA-980-1S 10min-10-95f 15 20 10MIN-POAA-9804S 10min-10-95f 16 21 10MIN-POAA-980-IS 10min-10-95f 8 22 10MI N-POAA-980-IS 10min-10-95f 92 23 10MIN-POAA-980-IS 10min-10-95f 17 24 10MI N-POAA-980-IS 10min-10-95f 18 25 10MI N-POAA-980-1S 10min-10-95f 19 26 10MIN-POAA-980-IS 10mirv10-95f 20 27 10MIN-POAA-980-IS 10min-10-95f 21 28 10MI N-POAA-980-1S 10min-10-95f 8 29 10MI N-POAA-980-1S 10min-10-95f 93 30 10MI N-POAA-980-1S 10min-10-95f 22 31 10MI N-POAA-9804 S 10min-10-95f 23 32 10MI N-POAA-980-1S 10min-10-95f 24 33 10MI N-POAA-980-1S 10min-10-95f 25 34 10MI N-POAA-980-1S 10min-10-95f 26 35 10MI N-POAA-980-IS 10min-10-95f 8 36 10MIN-POAA-980-IS 10min-10-95f 93 37 10MIN-POAA-98O-IS 10min-10-95f 27 38 10MIN-POAA-980-IS 10min-10-95f 28 39 10MIN-POAA-980-1S 10min-10-95f 29 40 10MIN-POAA-980-1S 10min-10-95f 30 41 10MIN-POAA-9804S 10min-10-95f 31 42 10MIN-POAA-980-1S 10min-10-95f 8 43 10MIN-POAA-980-1S 10min-10-95f 94 44 10MI N-POAA-980-1S 10min-10-95f 41 45 10MI N-POAA-980-1S 10min-10-95f 42 46 10MI N-POAA-980-1S 10min-10-95f 8 47 10MI N-POAA-980-1S 10min-10-95f 94 48 10MIN-POAA-980-IS 10min-10-95f 1 49 10MIN-POAA-980-IS 10min-10-95f 2 50 10MI N-POAA-980-1S 10min-10-95f 3 51 10MIN-POAA-980-IS 10min-10-95f 3 52 10MIN-POAA-980-IS 10min-10-95f 4 53 10MI N-POAA-980-1S 10min-10-95f 5 54 10MI N-POAA-980-1S 10min-10-95f 6 55 10MI N-POAA-980-1S 10min-10-95f 7 56 10MI N-POAA-980-1S 10min-10-95f 8 57 10MIN-POAA-980-1S 10min-10-95f 9 58 10MI N-POAA-980-1S 10min-10-95f 10 10 -- 10 -- 10 -- 10 -- 2 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 -- 10 -- 10 -- 10 -- 10 -- 10 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 QC 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 QC 10 -- 10 -- 10 -- 10 QC 10 -- 10 -- 10 -- 2 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard -- -- -- -- -- -- -- --" -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- --* -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- M assiynx - Sam ple List Sam ple List C:\MASSLYNX\Davey070799.PROVSampleDB\102799b.SPL Printed: W ed Oct 27 14:34:05 1999 File Name File Text 59 102799071 TOX145-RBS10229-1000ppb-1. RWW y P a g e Position: (1, 2) M asslynx - Sam ple List Sam ple Ust: C:\MASSLYNX\Davey070799.PRO\SampleDB\102799b.SPL Printed: W ed Oct 27 14:34:05 1999 / 'J '? 7 rage = Page Position: (2. 2) MS Pile Inlet File Bottle Inject Volume Sam ple Type Cone A 59 10MI N-POAA-980-IS 10min-10-95f 11 10 Standard FACT: DATA REYTEW SUMMARY FORM Date t/o s/tf Data Analyst: JS FACT Study : ~Ty( MS Matnx/Timepoints: P'g-v Sample Litt: Set-upAnalysis Date/Analyst Instrument Xa s SltLp Data Review Sign-OfT Analyst Review Name/ Date: ,. ______ . f , Technical Review . (los* < l d - f d / s / f i f a f f Name/ Date:_____ to h QualityAssurance Review Name/ Date:_________ Data Entry: _ (A c hIosIm Comments/Justifications: _____________ l' 2 We- Uljt Analyte: PoAA Ccm) AcceptableLinearRanee: AlA too. m ExtractionBlank: MA RA2: MA Matrix Blank: hJA CalibrationChecks AM MS/MSD: <J> MA DataStatus_ ________ LAC. Uosh*! ....... Analyte: T F oS C c ffz ') 0 AcceptableLinearRange: LOQ:. M f f L R-2: 0. ?t ?7? ExtractedBlank: /fe~ 00, Matrix Blank: //3S $4* dO . Calibration Checks: 0~ y f /ra*i - ? 7 o 9 ~ /? x o MS/MSD:_______ tM< - cat, ucJm. d \ L T / jlill rtp i-ifli Data Status: d s e.d 1.15 I W y x r . "H f fd t l t d /a, u si*. kJas t u f VUlA J a r ToA H I h J * . AS U S*t - r _ d r f t . ( p i e d 's aJ V e -J d i* - Jtm - J a s r t f a f a _______________________ LhJ e v tf QoaJ -, kAS k d ~2*- J j L t r J J * * - f i t . <y?^ r tc /ta * - U u J c . JLis- pfatt./ AMS jtduJtc/ Jfart 'fit. l'Ufo- 4o d / a A iTdKIf. fid M-dj k/Uhi Let*. &4/ii/ieg.K,-//j _____ ffccfof j bickeH'0Ujd IfjJe./*: of m Ii . --Jjls `l^'ff3oSs'U t (f^ ji Difycf Mbs tic cL d c J J > _ pvytoi'/dt a-Ldftr h f over J U iftnn a tr fd ju te Q .fp y ? n a -A JJe. d d a . - % s 'is/9<F Analyte: PFoSA FCHp) AcceptableLinearRange: ?3c>ol LOQ:____ B f&k ____ ExtractedBlank: IfS S Ma j i L Matrix Blank: (S i 4 it* L r i CalibrationChecks: OJt - A J e -f^ n \ ^ U " /a -- * ~ /3 % MS/MSD:____DK__________________ ^ IAC IIlashl DautSatus: Enle/tA_____ 5 m t (a o k \ t k Mi**- W ^ i l dl< U V \rc-l __________________________________ f\ rJis i**fa . A A FACT: DATA REVIEW SUMMARY FORM ` Data Review Sign-OfT D ale Data Analyst: Anelyat Review r / * Name / Date: 3 ^ 5 d/oS'n i FACT Study : Matnx/Timepointa: Sample Lit Set-up Analysa Date/Analyat Instrument: ____ _________ .________ Technical Review dSe,a_ - 21 Jrtt fiJ S>*/n/ - * d "hfft He# Name / Date:________ S o , jir. y . n a i /m u ____________________ ____ Quality Aasunaca Review Name / Date:___________________ "k iv i <*W 02o/?t Data Entry: lA C \ l ) c & e ci Commenta/ Justillcations: Analyte: * S n xr C c M ' ) ____________________________ _ AcceptableLinearRange: . LOQ:_____ h>A______ ExtractionBlank RA2 :______ U&______ Matrix Blank J k Calibration Cheeks A//I- M S /M S D :____________ A)A Data Status__________ Uh F t*-1 \M ulosh'l ( A ll/W ^ ^ 5 '</*/?f f ft I I *Ks l 9 t JNMMHH- soooooooooooooooooooooooc O O O O O O O O C >o o o o o c l i !P H * uhi p 300000000000000000000000 *O 1 0 J9 0 JHO^CO'JTlU'^UKIh iiiiiiiiiiiiliiiiiiiiiiiiiiiiiiif 1 EEiiEggElililllllisKO OK HOKrOKtO'KKOKHOKHOHOKHOKHOKHOr \W W W W U U W W W W W W KOM SU II OCM SIi SIi II -Ii II M10O..O... M- .O..O.O..O..O M M iN M M U M M l I IMM o I 1 1 oo ' . ~ ~ *3 M M *10 10 MMMMHMHMMMMM ooooooooooc MMWMMMMMMMMV O0O0000I000^ * lis SSS S S S S S S S i n oMO M- JoU mM oM oM wM oM aM M0 Mb MB O OKI " ' *011111 o u o w o o v o o- 8 B i-,, Rh o 53erSi SiSi T 7 10 7 10 10 _ m . S QSSS^ *0o w jrK er JT JT ? ? ^ filiv i ooeSS i i i er er II? S R " .filli T i <000 I Ml I IMM pHM * 5 S? OjjP*0' l -.-.--, f i SSSSr r ? . . s i & h i hsme e e- -I.:.:.:.-r-i-PSSr USSSSOIflOWs N L m 5 8 8 c c10<010 10 10 - M MM MM 5 i & S!H"2" ?I?I "H s ' :r n If i MM B m im SgBSS^ ^ V 10 M M M >0 >0 0S V X 00 10 *0 10 10 10 10 10 10 10 s s SS sss rftrfff*fTfr ill|l|l|| Laaaaaaat RS R MOMMMMMM MOM < o a m o w i 0 uiM o o ' U l U I O - J H - J i e v I OI m INW UW W 1 >4 U) W 0 O ) >1 I! >1 *1"J 4 -JJ N 1 J J 4 *J -J MMMMOM OMMMMMMMMMOO WM ( N<0 WH HU HH OpUk<l U4 IHHUHHKIaUaMKOIOUI%Oll > M O i | | | l 0 0 l>.IX V 553535353553 0UP 35 0k 10 M Ul L li 53353 553335 a 335333535333 B t O OOOOO OOOM )0<440UIUIft>4W r f 0 k l 4 I Mi 0 Ul ^l s G 0 t H> OMM O M M O O O 10 01 Oi M 01 O O J I 0 K I M 10 01 LH M 141 O OOOMOC 01 O M O 01 G UOU ^I 'OOMMUUgi BU 1 0l ' 4O0 >0 i~ 4 ' J lO 0 M 14 14 M I I* It l i s & ? e s MrMrrMrtMfIAfMnWnrItAfHT infilili aaaaaaaaa <0W M Sg-, ggggssgss nm S8 g ,g R g inuntatnwiaMM audilct 2sS 5 sggggsssss ? a* a I sS E sssssssasSp sspssS ssstssatSsscssSS sssassss? E5s2ss:s-oooo.S5SMslSs<.o,s,,ooasSsstsg->o<.o,oc.B S aSSSSg'gisE s'S55t:gggSgggbabiS5SSgggggg" :css5-5; CGCG5 S= o= i sss 3 siissis s s sii l O N n P 4 A o r * n n A 4 r t t O h 4 H O n h f i H n1 O ti O 4 B >iN044inininnitNit(iHNho>4inM4hnHn AM r * M n i n nnNrosrfr-sr>>einnMri'K.-itHnaHo< t 4 0 o l i >i n f i f iwn> 4NWf44 nnr4nrtNt>fir HA HNWH^ O H H O M HHHr' A )amrniAhMONvinrHn4iA4HHir4na)oBair4iAi<r ir4r<*iA<HiAr,>nnonoftn^nrst'mr*r'4rA,ir'ntnnnr-^r'>-<e>-ir'r>'or>g B -rf.r>r*r>rr *f'rf*r*r*r>rr'p*r o o o o a *: * 0 HO S3 as 1< 1L1L tf | | * N 0 4 H BH H 0 O O O < _ Nh n4 I! hisiA ^ O m * e - o s L L H gogo H H n s e O IJ Mi* * I t h ;j ? O u M M M ..>i2 3Jjlj i II lm fil! UUUU MWVI M a MbMbMkChH lillli asa aa 30 o o a oo oo a: B *** 8 nnn OOOOO OOA IN S S S VVf o n n n n * n n aa as - m *...HBN.A.NHB..Af..f.Vl..J'..i..p..0Sf..fN0..lA.0S.A.V0..AV.0.SO'A*.s'.<.S.s'nfA.s) SSSSSA ......... a ** ss- HHNAAANSNSH -NHHHHHHH -- JJJJj M*** *.!f|*. | | 8 . - mS S U S S S 8 S S S S *-' s s ? " a ? ? , J I H H l i t H.. n il l1 iisA l s.Q J3 OhbaKSSooo BV V BOn OOW O ^j-gggsssas^ jiiiiiii i M M - . O V* O O t J< H H I I I I J i 5 S s s s 1 3 s s 3 S I ^ ^ s I ^ E 13 E s | t S a a s r s s s s's *** t f l V f l i A A A A l O i A A A A i B l A I A V A A m i A V i A M A l A A M W M d A A A n A A A A A l A l B A A A i / l l / ) - H oH5nSH 88on2rto3H$ilK ^K B!****^^3^*****^* ; iiieggeffeegeggiegeppeigggggieegigegggggpggg B h B Bl O H IS i . . ........................... 5 0 0 00i 0H0HCr t5M--0---N-C--A----M-----N N O NNM OOO NAAAAi-. OOOOOO C >o o o c _B iB iB iB iB ltlB lB iB lB iB iB iB iB lB lftA B lB lB lB lB lA B IB lA B lB IB iB lB \B iB iB iB lB iB iB lB lB lB lt OOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOC Misn/Mfa^OHr4r V : i %it I ? S a " " S a 'S ', " ''" |iiS S ', 3 "'S r' 3 rr 3 5 7 ''T'?g3,T S2'rT a77<'r3 j a a s s s a s s s s s s g s s s s s s s ^ ^ a s s s s g s s s s s s s s s s s s 5 H H H H H H O H H rtH H O O O O H H rtO H W O H H O < -4 0 0 0 0 0 0 0 0 0 0 0 0 r -I Q O a a a a a a a a a a a a a a n a a a a ia a a a a a aan a ssa sa a n a sa ia i 5 lslliSgs2l3ISSssa=slls sirslssllsllsls 5 g S 3 3 5 S53S3=SSESa5SSSSa s H S S s s s l I H S ; *- r->rrr-r'rr'r->r>r'rr*r'>rr'>rrtr*r'-rr*r'Fr-*r- rrr*rr*r*r-ff-r-rr" r'f'rr* SSggggggg g gg ggggggggg H HH r4H H F lH H r(H H fl' ?r" & a I a 1 ! i T a* "IoSff? y )* H ri i ep 0301: Quaaelt*c ad prlsccd toy 1* 11/05/ loup 030199: Q u u t l U t a d u d prlaetd toy l u OA 11/0S/99 > 3 oop 020199: Qunelettad sad prlatad toy l u eo 11/05/99 Quantify Calibration Baport TOX14S-rat aora, day 39 doi< itrol- oat- 11/3/99 Compound 4 name: Sun (Ch4) Response Factor: 2153.97 Response type: External Std, Area Curve type: RF 2.54e3-i fag* 4 X XX * XX XX Soup 030199: Quaacltatad and prlntnd by laa 11/09/99 Method port Method fila : L u t Modified: Coapound: Printed: C :\M A S S L Y ia \e o u p 0 2 0 1 9 9 .p ro \M a th D E \1 1 0 4 9 9 e .M d b Pri Mov OS OS j29 1 44 1999 It PCA (CM) Pri Mov OS 04:54:56 1999 Coapound N a m : Internal Raf.: Quantify Traa: Cone, of Standard#: Dear RP Valua: Otar Peak Factor: Integrate window Factor: Chramtograa m a a window: POAA (CM) (Mona I TIC Fixed 1.000000. Disabled 1.000000 2.000 l.OOOODa Rataation Tima (mina): Relative Rataation Tima: RT Rafaranca: T i m Window (mina) : Paak Selection: 7.167. Enabled 0.000. Disabled (Mo m ) 0.345 Nearest Raaponaa Type: Raaponaa: External Axe u Polynomial Type: Point of Origin: Pit Weighting: Axis Transformation: Linear feccluda 1/X Mo m Oaita: Paak>to-peak amplitude: 11 Seoo thing: Window site (scans): R e b a r of mooths; Seoothing nethod: Enabled 2 1 Join valley threshold: Reduce peak tailing: Raise baseline -- r iwm: Draw vertical threshold: Detect shoulders: Shoulder threshold: Ralativa height: Absolute height: Relative area: 10.00 200.00 S.00 90.00 Disabled 20.00 1.S0. Disabled 0.00. Disabled 2.00, Diaablad 0.00. Diaablad 'U * " h f o f Uf Pag 1 Method file: U i C modified: rfcinnnil Printed: C :\M A S S L T J IX \a o u p 0 2 0 1 9 9 .p ro \lle th D B \li0 4 5 9 a Pri M e v 0 5 0 4 : 2 9 : 4 4 1 9 9 9 2: pros (Ch2) Pri Hov 05 04:54:54 1999 Ccnpound Nana: Internal Ref.: Quantify Trace: Cone, of Standards: Osar HP Valua: Osar Peak factor: Integrate Window Factor: Chromatogram aasa window: Retention T in a (mins): Relative Retention Tina: RT Reference: Tina Window (nina): Peak Salaetion: Raaponaa Typa: Raaponaa: Polynomial Type.Point of Origin: Pit weighting: Axis Tranaformation: pros <ch2 ) TIC Cone. A 1.000000, Disabled 1.000000 2.000 l.OOOODa 7.429, Enabled 0.000. Disabled (Won] 0.447 nearest External Areas - Linear Exclude 1/1 hone Units: Peak-to-peak aa^lituda: &aoething: Window aise (acana): Munbar of smooths: Smoothing method: Join valley threshold: Reduce peak tailing: Raisa baseline maxiaui: Draw vertical threshold: Detect shoulders: Shoulder threshold: Relative height: Absolute height: Relative area: Absolute area: 1 Enabled 2 1 30.00 200.00 5.00 90.00 Disabled 30.00 . 1.50. Disabled 0.00, Disabled 2.00. Disabled 0.00. Disabled Method Report Method file: Last Modified: Compound: Printed: C:\MASSLYHX\aoup020199.pro\MethDl\110499a.mdb Pri Nov OS 04:39:44 1999 3: PFOSA (Chi) Pri Nov 05 04:54:54 1999 C a b o u n d n m : internal Ref.: Ouantify Trace: Cone, of Standarda: User RP Value: User Peak Factor: integrate Window Factor: Chromatogram mass window: Retention Tine (nine): Relative Retention Tine: RT Reference: Tina Window (nine): Peak Selection: FFOSA (Chi) (None) TIC Come. 1.000000. Disabled 1.000000 2.000 l.OOOODa 1.147, enabled 0.000. Disabled (None) 0.554 Nearest Response Type: Response: external Arasa Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Linear Exclude 1/Z Hone Units: Peak-to-peak solitude: 1 Smoothing Window sire (scans): Number of smooths: Smoothing method: Join valley threshold: Reduce peak tailing: Raise baseline aaximm: Draw vertical threshold: Detect shoulders: Shoulder threshold: Snablad 2 1 30.00 200.00 5.00 90.00 Disabled 30.00 Relative height : Absolute height : Relative area : Absolute area: 1.50. Disabled 0.00, Disabled 2.00. Disabled 0.00. Disabled Peg* 3 Method Report Last modified: Compound: Printed: C: \HkSSLTWX\soup020199 .pro\NethDE\110499e.mdb Pri Mov 05 04:29*44 1999 4: Surr (Ch4) Pri MOV 05 06:54:54 1999 C o m o u n d Ma m : Internal Ref.: Quantify Traca: Cone, of Standards: Usar HP Vala: User Peak Factor; Integrate Window factor: Chromatogram m a a window: Surr CCh4) (Mom] TIC fimd 1.000000, Disabled 1.000000 2.000 l.OOOODa Retention T i m (nina): Relativa Retention Tim: RT Reference: T i m Window (nine): Peak Selection: Response Type: Response: Polynoedal Type: Point of Origin; Pit Weighting: Axis Transformation: 7.211, Rnabled 0.000, Disabled (Mom) 0.379 Nearest Xxtemal Areas Mnsir Exclude l/x one Oaite: Peak-to-peak amlicude: 11 Smoothing: Window size (scans): Number of smooths: Smoothing method: Enabled 2 1 Join valley threshold: Reduce peak tailing: Raise baseline maximum: 30.00 200.00 5.00 Draw vertical threshold: Detect shoulders: Shoulder threshold: 90.00 Disabled 30.00 Relative height: Abaolute height: Relative area: Absolute area: 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled . Png* 4 Quattro n, #6414E ' SOUP 020199: FACT Equipment Log 99092 PAGE VI DATE: 11-04-99 S S erM I MATRIX: rat ser_a_DESCRIPTION- day29- dose & conggj FACT Method: ETS-8-5.1 Injection volume: 10 uL Cycle time: IQmin, Electrode: Z-Scai Mobile Phase: ` n mMNH4CH3CQ2 mi MeOH TN-A- or stndrdnumber (A) 90085-11-15------------ m iTN-A-2997 Prepared (date/by): (A) 10/30/99 sab - mi 10/30/99 sah Expires: (A) 04/Q0----------------------- m i 2010 Storeatroomtemp? 0 or N Other:-- Guard column: None ________ ____ Part number: na_______ Lot number:_na. Analytical column: Size:2 x 50 m m _________ ____ Type: Cl?------ Part nnmher: 055-701-2________ Lot number: P9H i Sphere size: 5 urn_____ Serial number:0591804Z Analytical parameters: Drying gasHThrl: 350 ESI nebulizing gas(L/hr)_U----- Sheath gas (L/hr)JL LC Flowrate: 800uL/min. Back pressure: $5 bar_ HPLC solvent gradient: 10min-10-95 Time (min.l DJLQQ____ 2)_LflQ____ 3LL5Q___ 4 )7 ^ 0 ____ 51 8.00 %B 10.0 1 M ______ 95.0 _ 2 1 Q ______ 1 M ______ T u n in g M ethod R e p o rt M ethod: c :\M A SSLY N X \SO U P020199.PR0\ACQUDB\PF0S3 P rin te d : Thu Nov 04 1 4 : 0 2 : 2 7 1 9 9 9 SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. S et Rdbk 1.60 40 5 0.2 150 250 1.62 -41 -7 150 250 P re ss u res Analyser Vacuum Gas Cell Rdbk 5.le-5 4.Oe-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier S e t Rdbk 14.0 14.0 0.9 0 .0 4 650 3 MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier S e t Rdbk 14.0 14.0 10 2.0 0 .0 40 0 650 7 36 1 '* . m b b Iv Mstbod M p o r t wuud: cn>nM.Mtt*a<>oaoit.*ovcwDuoii-**o-0 *-" 0 " 'Ii >..> Modified: Prl Oct IS 10:35*03 1**9 friMid: Tta Bpv 04 13:10*30 1999 Solvent Dalay ( aloa ) : 0.00 Function I 1 M W of 1 Maas Pair ( f * ) Xoesr ttannsl Daisy ( Sacs ) : Spaa ( Daleona > : scare Tine ( Mias ) t Bnd Tine ( Mina ) t 0.03 0.00 0.00 10.00 R-P* tQannl Parane Daughter Dwell (Sacs) Coll tnargy (aV) i 113.00 149.00 0.30 30 Con# ( V ) Function : 3 m of 1 Maas Pair ( B*P> ) Incar Cbannsi Dalay ( Sacs > : Span ( Daltons > : Start Tine { Kins ) : Bad Tina ( Kins ) : 0.03 0.00 0.00 10.00 **P"*tCtannel Pnrsnt Daughter Dwell *Seca> Coll Snarpy (aV) Cons ( V ) 1 499.00 99.00 0.30 .45 40 Function * 3 M W of 1 Mass Pair ( * - ) Intar Channel Dalay { Sacs ) t Span ( Daltons ) i Start Tine ( Kins ) : Bnd Tina ( Mins > : Repasts : Channel Parent Daughter 0.03 0.00 0.00 10.00 Dwell (Saco) Coll laargy (aV) Cons { V ) 1 49.00 78.00 0.30 45 * Function : 4 I of 1 1 aa pair ( : Inter Channel Dalay { Secs ) s Span ( Daltons ) : Start Tine ( Kins ) : Bnd Tine ( Mins ) i C b i s M l r u n t Daughcar 0.03 0 .0"0* 0 .0 0 10.00 1 D~ll <Saca) Coll narsy (aV) Cona ( V I 437.00 0.00 1 Method Report Method riles L u t Modifiedi printedi CI \MASS1TOX\SOUP020199 . PRO\XC<JUDB\10min-10-95 Tbuzaday, Noveaber 04/ 1999 Ils22s29 Thursday, November 04/ 1999 13 il8 :38 HP1100 1C pump I n i t i a l conditions Solvents A% B% C% D% Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Let(C) Oven Temperature Right(C) 90.0 10.0 0.0 0.0 0.300 10.0 0 400 30.0 30.0 HP1100 LC Pune Oradiant Timetable The gradient Timetable contains 5 entries which are Time 0.00 1.00 5.50 7.50 8.00 A% 90.0 90.0 5.0 5.0 90.0 B% 10.0 10.0 95.0 95.0 10.0 C% 0.0 0.0 0.0 0.0 0.0 D% 0.0 0.0 0.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 HP1100 1C Pune external event Tiaatabla The Timetable contains 3 entries which are : Time Initial 0.00 0.10 Column Switch Contactl Off Off Off On Off Off Contact2 Off On Off Contact3 Off Off Off Contact4 Off On Off HP1100 Autoaaavlar I n i t i a l Conditions Draw Speed Eject Speed (pi/min) Draw Position (mm) Stop Time (mins) Injection Volume(pi) Vial Number 200.0 200 0.00 9.00 10.0 51 Pressure 400 400 400 400 400 Masslynx - Sample List , Sample List: C:\MASSLYNX\soup020199.pro\SampieDB\110499a.SPL Printed: Thu Nov 04 13:18:22 1999 Page 1 Page Position: (1,1) File Name File Text MS File 1OMIN-PFOS-POAA- PFOSA-IS 1 110499001 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 2 110499002 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 3 110499003 MeOH Blank ,,,, 4 5 6 110499004 TOX145-RBS11039-H2O Blk-9, ext. 11/39 MCH 110499005 TOX145-RBS11039-Sera Blk-9, ext. 11/3/99 MCH 110499006 TOX145-RTS1 1039-Sera Blk-9, ext. 11/3^9 WOH 7 8 110499007 TOX145-RBS11039-5ppb-9, ext. 1 1 ^ 9 MCH 110499008 TOX145-RBS1 1039-10ppb-9, ext. 11/3/99 MCH 9 110499009 TOX145-RBS11039-25ppb-9, ext. 11/3^9MCH 10 110499010 TOX145-RBS11039-50ppb-9, ext. 1 1 ^ 9 MCH 1 1 110499011 TOX145-RBS11039-1 OOppb-9, ext. 11/3/99 MCH 12 110499012 TOX145-RBS11039-250ppb-9, ext. 1 9 MCH 13 14 15 110499013 TOX145-RBS11039-500ppb-9, ext. 1/39 MCH 110499014 TOX145-RBS11039-750ppb-9, ext. 11/39 MCH 110499015 TOX145-RBS1 1039-1000ppb-9, ext. 11/3/99 MCH 1OMIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 1OMIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 1OMIN-PFOS-POAA-PFOSA-IS 1OMIN-PFOS-POAA--PFOSA-IS 10MIN-PFOS-POAA'PFOSA-IS 1OMIN-PFOS-POAA-PFOSA-IS 1OMIN-PFOS-POAA-PFOSA-IS 1OMIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 110499016 110499017 110499018 110499019 110499020 110499021 1 10499022 110499023 110499024 110499025 110499026 110499027 110499028 MeOH Blank TOX145-RTS11039-250ppb-MS9, ext. 11/3/99 MCH TOX145-RTS11039-250ppb-MSD10, exL n ^ 9 9 MCH TOX145-RTS-9R03240M-0-Day 29, ext. 11/3/99 MCH TOX145-RTS-9R03241 M-O-Day 29, exL 11/3/99 MCH TOX145-RTS-9R03242M-0-Day 29, ext. 11j^99 MCH TOX145-RBS11039-250ppb-CCV9, ext 11/3/99 MCH MeOH Blank ,,^ TOX145-RTS-9R03243M-0-Day 29, ext. 1 1 ^ 9 MCH TOX145-RTS-9R03243M-0-Day 29, ext. 11/3^9 MCH TOX145-RTS-9R03255M-5mg/kg-Day29, ext. 1 /3/99 MCH TOX145-RTS-9R03256M-5mg/kg-Day29, ext. 11/3/99 MCH TOX1 45-RTS-9R03257M-5mg/kg-Day29, ext 11/3/99 MCH 1OMIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA- PFOSA-IS 10MIN-PFOS-POAA--PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA'PFOSA-IS 10MIN-PFOS-POAA--PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 110499029 TOX145-RBS11039-250ppb-CCV10, ext. 11/3/99 MCH 110499030 MeOH Blank ,, ,, ,, . , , ,, (no , . _ u 110499031 TOX1 45-RTS-9R03258M-5mg/kg-Day29, ext. 11/3/99 MCH 110499032 TOX1 45-RTS-9R03259M-5mg/kg-Day29, ext. 11/3/99 MCH 110499033 TOX145-RBS11039-250ppb-CCV9, ext. 11/3/99 MCH 110499034 MeOH Blank 110499035 TOX145-RBS11039-H2O Blk-9, ext. 11/3/99 MCH 110499036 TOX145-RBS11039-Sera Blk-9, ext. 11/3/99 MCH 110499037 TOX145-RTS1 1039-Sera Blk-9, ext. 11/3/99MCH 110499038 TOX145-RBS11039-5ppb-9, ext. 11/3/99 MCH 110499039 TOX145-RBS11039-1 Oppb-9, ext. 11/3/99 MCH 110499040 TOX145-RBS11039-25ppb-9, ext. 11/3/99 MCH 110499041 TOX145-RBS1 1039-50ppb-9, ext. 11/3/99 MCH 110499042 TOX145-RBS11039-100ppb-9, ext. 11/3/99 MCH 110499043 TOX145-RBS11039-250ppb-9, ext. 11/3/99MCH 110499044 TOX145-RBS11039-500ppb-9, ext. 11/3/99 MCH 110499045 TOX145-RBS11 039-750ppb-9, ext. 11/3/99 MCH 110499046 TOX145-RBS11039- 1 000ppb-9, ext. 11/3/99 MCH 10MIN-PFOS-POAA'PFOSA-IS 10MIN-PFOS-POAA'-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA PFOSA-IS 10MIN-PFOS-POAA -PF O S A -IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA'PFOSA-IS 10MIN-PFOS-POAAPFOSA-IS 10MIN-PFOS-POAA -PFOSA-IS 10MIN-PFOS-POAA -PF O S A -IS 10MIN-PFOS-POAA- PFOSA-IS 10MIN-PFOS-POAA- PFOSA-IS 10MIN-PFOS-POAA- PFOSA-IS 10MIN-PFOS-POAA' PFOSA-IS 10MIN-PFOS-POAA'PFOSA-IS Masslynx - Sample List ; Sample Ust: C:\MASSLYNX\soup020199.pro\SampleDB\110499a.SPL Printed: Thu Nov 04 13:18:22 1999 ' ; V ; ' ' 1 '.'A .. Inlet File B o ttle 1 10min-10-95 91 2 10min-10-95 91 3 10min-10-95 91 4 10min-10-95 1 5 10min-10-95 2 6 10min-10-95 3 7 10min-10-95 4 8 10min-10-95 5 9 10min-10-95 6 10 10min-10-95 7 11 10mir>-10-95 8 12 10min-10-95 9 13 10min-10-95 10 14 10min-10-95 11 15 10min-10-95 12 16 10min-10-95 92 17 10min-10-95 13 18 10min-10-95 14 19 10min-10-95 15 20 10min-1O-95 16 21 10min-10-95 17 22 10min-10-95 25 23 10min-10-95 92 24 10min-10-95 18 25 10min-10-95 19 26 10min-10-95 20 27 10mirt-10-95 21 28 10min-10-95 22 29 10min-10-95 26 30 10min-10-95 93 31 10min-10-95 23 32 10min-10-95 24 33 10min-10-95 25 34 10min-10-95 93 35 10min-10-95 1 36 10mirt-10-95 2 37 10min-10-95 3 38 10min-10-95 4 39 10min-10-95 5 40 10min-10-95 6 41 10min-10-95 7 42 10min-10-95 8 43 10min-10-95 9 44 10min-10-95 10 45 10min-10-95 11 46 10min-10-95 12 Inject Volume Sample Type Cone A Cone B 10 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- _ _ _ _ _ -- _ _ -- _ _ _ _ -- _ _ _ _ -- _ _ _ -- -- _ -- ~ -- -- _ -- _ _ -- -- - ~ -- -- -- -- _ -- -- _ -- -- -- -- -- _ _ -- --- -- -- " _ -- -- -- -- -- -- -- -- -- _ -- -- 10 -- 10 -- 10 -- 10 -- ---- _-- _-- ---- Cone C -- -- -- -- -- " -- -- " -- -- -- -- -- -- -- -- -- " -- -- -- ~ -- -- ~ ~ " -- -- -- -- " " ~ -- -- - Page Position: (2,1) FACT: DATA REVIEW SUMMARY FORM Date DataAnalyst: JS FACT Study*: 75*/Vc Mstrix/Timepoints: t- <U j 3 9 f t / t f n l j / t * . ~~ f? /? 7 Sample List* Set-upAnalysis Date/Analyse Instrument f o t t i ------------------------------------------------------ M ff t/o s -M nom Analyte:. 0P<*M Caff') AcceptableLinearRange: tf* LOO: fJA_______ ExtractionBlank: HA. RA2:_____ M _______ Matrix Blank b/A CalibrationCheeks: HA MS/MSD: U lfr 3 DataStatus: ~j?Arfa/gL-^L^gjkiL- Analyte: Tfes C(H z')0 AcceptableLinearRange: LOQ:. Vf-tO vnb ExtraetedBlank: fa s -JIa a . QQ R A2: 0.191 Matrix Blank &&*. 0Q CalibrationChecks: OP ~ MS/MSD: ______________ DataStatus: (b t a J T V lk -C / .Ml Wio Data Review Sign-Off Analyst Review . Name/ Date: 3*c 'U ffa Technical Review f . , -, Name/ Date: H H Z? l i h / O 1^ fijh h W - g ~ 7 ? QualityAssurance Review Name/Date:_________ Data Entry: Ulfeiffi Comments/ Justifications: C t f i / r d l t Us&S ttA~f KtA- 7&AA. P UStL L y r& - fd s L ^ 7 * * - -fju * J/C L . - & * * / * ( 9 f. Q. 777 LoukJ (u .n x *a/~ f-? 3 j> /r a r . c f ?-7tf> h M r , C r r L J g J L j * r t f U iN - fU - Z o " / 6 r ta .r a (tj ' ^ u J rrK L iu h f 'fU m d L J iJ iM -J L P k -n ^ s b x r * .------- I O L K r <L i h j a u r o m A s y pXr>*rj**tL* t t J ( 4 L Ljo u - j * s > /a /r T U r J J J A ree- Caun-r S -* -p /,C J u t r t f u (fu * -lo 't< - J t L f o * . 'f o j o r 5 " fr 9 9 Analyte: TFoS A ( C H i } AcceptableLinearRange: -9 3 & oL ' ft? p jJ u LOQ: ExtractedBlank /(S s f* * lO Q R-2: D - i m O Z Matrix Blank !* S s -ilia .* . C*X CalibrationCheeks: OP ~ j .___________________ MS/MSD allf1- DataSams: l j a h a l fatn p n j . M - FACT: DATA REVIEW SUMMARY FORM Dale: f'/o s iff Dau Analyst: JA S ___________________ ___________ FACT Study$ fo i N S _______________ ________ Mitrix/Tirnepoints: v i e . . - L , tv d ,i* . 1 f i a t - L / - t o t W f t SamplLift II 0 * 1 9 o ____________ __________ Set-upAnalysis Date/Analyst: N * u 'k i n - _________________ instrument: y> Q2ol99 - . Analyte: S u n f o i l ) Acceptable Linear Range: AM LOO A_________ R-2: /la CalibrationCheeks m MS/MSD:_____ DataStatus Extraction Blank: Matrix Blank: . Data Review Sign-Off Analyst Review Name / Date: // l tl9 Technical Review Name/ Date: f h t r __pPM.- > LLQualityAssuranceReview u c uhfa Data Entry: l?> Lr k Comments / Justifications: ---- 0 ----- [ A c u h l w It It i l l S 5 l t t B m i MtnttMUMttttta S iv m sss ? 'r r s l <1g<4 s|<4*4g<4<4Mglg<4>4j<4g 5S55ESH5SS5 SS5SSS ggS&SSSSSSSSSSi S 3 S S 5 P C P 3 5SKSKS 5S3 C5SSCS5S5SS m m m m m m m issm m m s k s s s s s k b s s s sisksbi: s b s s k s s k rk k is s k s * =,,3 B S 4 . " tiSf -P s w ! B(OiOV>r4ni>iOr* )>i4 o o N 4 mn r Oit V, -.-1 t f - > n N O .hl-/Tn.aO oOoooOnr I4 i/MS n h r 'f> 4 n K 1 r < O Q O O ' M i n W 4 4 r 1 l iiiOwn m rtriinnori>4)hr< iiili l (444l99ilAVHr^HnfOONriOOS0VHn<4VO^41A 4i i nnHNr i n Aii h >efM*4nhnnnhe MH norniaHohHHf 4 4H r44tho OrH>m ro mro)c4o nMN h h h Hn S4 0 f f l 4 0 4 1 4 M r t l * O O m Q i n H 4 H n M | . M 0 4 4 l i n O r t nrtnniinnrtrM4r4ni4nr4rtnnnnnnn4nfii4(it4iii4<4Nfir n 4 A 4 >n r i l HH 'O u r n * Iwji la!a * !i I.i *>4*l H* 4WOH H fl M **4 l I&i= IMJ 1 Ai fi ljli i H filli i SLsisS!!? I il.ssssss! A^ V ^ f i mt * mi ao *o**o**O* o* _m ^o s s ] w nvNn*i*' J h 3 ? T AAAA a"o .mluAa oagiagAoioigoo 4goigooogncel oooooooooooo f i n 14 III .! ! ! 3 Siiti . h s s k l ... . '0t0t9l> I liim * 4 i a ai ai ai AaS ajSqaiabaAcaSoa, 4KK4Kc5 5 S S rn*>nrm*trnnirr*in*f*rin<i4 B_ H.|. I.i. Inaf)oHatNaf t4oAo>o4tNen omowo^tooH O O o O O ri n n n.n..n.n..n..n.ninm nrnm OOOOOOOOOOOO 11133e3333333331E3S3133B333333333 iifiBifiifiBininifiMii/nifiniw >? 5 ? a 3 3 a a a g a a g 3 a g a s g a a g g 3 s a a a a H 3 3 a a g8egB8epgeBglpggeegggEeeee88BeB oooooooooooooooooooe'U-k----9i--9i--B--9-i--I-------- -- - l 4 h a 9 i O H N I al 4 M W h B \ O H r o^nin l a n e o o o 4 9 i n o ' ,i m r M H n o o o e e o o o e 4 0 4 t 4 H < * n N n h N 4 r<> ! 4 I0 9 IH Iim illlll9 1 1 lililIilll ni/iwwf-M Hnin>4h<t ssa: *rr*r-rr-r-fh 'rr*rtrfr~frr*tpr*r*p-r'ph oooooee Mheeeoooo It4 K < k A h 1h f> TOX14S-RSU039-1000ppb-9, xt. 11/3/99 nMuinMuiin Ii !* L i. # * ! . e i " g; ' M>4ir IsB: ! ] ,?8 B! ? Or : ! !i iijij i Si Illll ssgSSS8858! ? **n n h k k k k k s a h h h a n Asi s NfVt.<d wd d^snN^s Mv n-V. Q Q.Q..QhQ.Hh HH H H S rA t^lSANi^A H- srStNHSHH . . . . . . . 0. 0101* 01 li `t H H ^ n NNN N 8 gSSS88888 n n n ddddddd ns sH sH dddNnNksinNns nv Av H H H ANSAN SA rAtWr ISHSH iSHHHHHHA illHAHH !" < !!! Hls ! m ii. O ki li a a S a o g e o e XX i l i l O Mw^0>n aa.-iu i nOh hUS5a M aS p uo i e i o f o ................ O..O..O..O...O..<-.i...A-n.n A A A n A A f l A > 0 0 0 0 0 0 0 0 0 0 KKKKUo o o o o o o o o o o o MltHintAlAlAlAlAiniAiniAtniAMlA^lA^lAinNlAlAyllAlAlAl/IVIVI^in I2?353333333323g333333s3g333333233 ^^igBeeeeeegeeBeeeeegegggegegee Od Od dO dO dOdOdOdOdOdOdOdOdOdOdOdOdQdOdOVOiOdOdOdOdOdOdOdOdOdOd Od Od dO dO oC idddddddddddddAdddddddddddddChdddddt iminvDAintntiHniAininknAtftM^iinviiAMMiA^iniAMMiAniAiniAdiAi/ O O O O O O O O O O O O O O Q O O O O O O O O O O O O O O O O O O O C ! I QttMtUy G r o u n d r Mport control ami oaa- U K ! CMtKlLnttNKUpOaOlf.pKVla^lKBVilOSflto Lase odi fiad: fri It o * 05 15:24:11 1555 Vf- n , i a M t t MacLod: C:\lttS8LTllXSsoup020159 .pro\llath\110S99b Ult wxUCiad: Mas Mov 00 07:09:90 1* job Coda: Fristad: Moa or 04 07:20:42 109 n i m i n l 4 1 Surr (Cb4) Mama 1 11059902B 2 110599029 3 110599030 4 110599031 5 110599032 6 110599033 7 110599034 8 110599035 9 110599034 10 110599037 11 110599030 12 110599039 13 110599040 14 110599041 15 110599042 14 110599043 17 110599044 18 110S9904S 19 110599044 20 110599047 21 110599048 22 110599049 23 110599050 24 110599051 25 110599052 24 110599053 27 110599054 28 110599055 29 110599054 30 110599057 31 110599058 32 110599059 33 110599040 34 110599041 35 110599042 SMelalse Taxe HaOK Blank MeOH Blank MaOH Blank m TOX145-RBS110J9-IC0 Blk-9. t . 11/3/ TCXU5-BSn39-Sr Blk-9. K . 11/3/" ~ TOX115-RTS11039-Sr Blk-9. ' 3 1 / 3 / 9 9 ICH TOX145-RBS11039-5ppb-9. axt. 11/3/99 TOX145-RBS11039-10ppb-9, axt. 11/3/99 1 TOX145-RBSll039-25ppb-9. axt. W TOX145-RBS11039-50ppb-9, axe. 11/3/99 I OE TOX145-RSll039-100ppb-9. axt. 11/3/99 TOX145-RBS11039-250ppb-9, axt. 11/3/99 M TOX145-RBS11039-500ppb-9. axt. 11/3/99 M TOX145-HBS11039-750ppb-9, axt. 11/3/99 M TOX145-RBSU039-1000ppb-9. axt. 11/3/99 KaOH Blank TOX145-RTS-9R03255M-5xc/ko-Day29. D:10 TOX145-RTS-9R03256X-5B/kg-Day29. 0:10 TOX145-rrS-9*03257M-5ao/kp-Day29, 0:10 TOX145-RTS-9B03258H-5aff/k-Day29. 0:10 TOXH5-*TS-9*03259M-5B/ko-D.yI9. D.10 TOX145-RBS11039-250ppb-CCV9. axt. 11/3/99 W S KaOH Blank TOX145-RBS11039-H2O Blk-9. axt. 11/3/99 I TOX145-RBS11039-Sera Blk-9. axt. 11/3/99 MOI TOX145-RTS11039-Sara Blk-9, axt. 11/3/99 ICH TOX14S-RBS11039-5ppb-9, axt. 11/3/99 I O ^ TOX145-RBS11039-10ppb-9. axt. 11/3/99 I O TOX145-RBS11039-25ppb-9, axt. 11/3/99 = TOX145-RHS11039-50ppb-9. 11/3/99 TOX145-RBS11039-100ppb-9, axt 11/3/99 TOXl45-RBS11039-250ppb-9. axt 11/3/99 TOX145-RBS11039-500ppb-9, axt 11/3/99 TrOoXxli4455--RRBSS51i1i0u3j9--7/S30wppppb--9, ah-xt-. 11/3/99 jOXl45-RBS11039-1000ppb-9, axt. 11/3/99 Stilalard Standard Standard Standard Standard Standard seandard Standard Standard QC Standard Standard Standard Standard Standard Standard Standard Standard Standard HT 7.189 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 7.171 7.148 7.147 7.141 7.109 7.149 7.169 7.126 7.100 7.167 7.168 7.146 7.124 7.165 7.189 7.190 7.192 7.187 7.191 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 7.150 7.193 7.127 7.167 7.142 7.136 7.164 7.141 7.147 7.147 7.168 7.125 araa Flava 15 bb Cene. bona 0.01 -99 1783 bb 2054 bd 1850 bd 204t bb 2244 bd 2181 bb 1S40 bb 2250 bb 2303 bb 2399 bb 2114 bb 2021 bb 10 MI 244 bb 244 bb 249 bb 253 bb 234 bb 2199 bb 2009 bb 2498 bb 1954 bb 2085 bb 2249 bb 2233 bb 1846 bb 2432 bb 2147 bb 2280 bb 2135 bd 1983 bb 0.83 -17 0.95 -5 0.86 -14 0.95 -5 1.05 5 1.01 1 0.85 -15 1.04 4 1.07 7 1.11 11 0.98 -2 0.94 -6 0.00 -100 0.11 -89 0.12 -SS 0.12 -SS 0.12 -88 0.11 -19 1.02 2 0.93 1.16 0.91 0.97 1.04 1.04 0.86 1.13 1.00 1.06 0.99 0.92 -7 16 -9 -3 4 4 -14 13 0 6 -1 -8 Soup 020X99: Quantitatad and printad by ina oa 11/08/99 -M-s . /./y t Soup 020119 Qu*f)tlCt*4 ad printed toy l u n 11/00/99 Soup 020199: Qunatltatad ad printed by ina on ll/Ot/99 P*9* 3 o o p 020199: Quaatlt**d and printed toy l u 11/00/99 l0t 4 loup 020199 : Qu*Atltit*d tad printed toy !* oa 11/0/# Kethod R iport Mcchod i . f . L a it mcd . `.a d : C:\Ny ".LYTn<\seu? c :0 1 9 9 .pro\M ethD S\110599b.m db Men *w Ci 3 7 :C ?:3 3 199 Compound. p rin ted ; ** Cn.) K .n OJ 27:2}-.U 1999 _________________ Compound Name: Internal ?..: Quantify Traea: Cone, of Standards: User RF Value: User Peak Factor: Integrate window Factor Chromatogram mass windov: pc.^ :chi) Fixad 1.00C300. Disabled I.O0C300 2.oc: i.c::JDa Retentier- Time (mir.. Relativ* ,cention RT Refer- re: Time Wir * (mins); Peak Selection: Response Type: Response : 7.1*:. Enabled 7 .::: . Disabled 3.2C2 1 Polynomial Type: Point of Origin: fit Weighting: Axis Transformation: Linear Exclude 1/X Nere Units: Peak-to-r -s< amplitude. Smooth ir; Window s .:e (scans): Dumber c r smooths : Smcothir; rethod: Join vail ay threshold: Reduce p y*. tailing: Raise baa ilir.e naxur.ua: Draw vert ;cal threshold Detect sr.raiders: Shoulder threshold: area: Absolut -* tea : 1C j r.-.allid - ;c.:: *''` 90.:: Disacled 30.c: 1 .5 7. Disabled 7.13. Disabled l.CC. Disabled :.::. Disabled tfc i " U f a P- M f ' Pege 1 Method R*;ort Method file: best noddled: Compound : Printed: CtUL-.SSLTrc'.soup^aiM. pro\MethOB\110S99b.mdb von ::.'V 08 Cir.i.il 1999 2: P:Z5 (Ch2: Mon :::v 03 :7; 23: 54 1999 Compound Name : Internai Re.: Quantify Trace: Conc. e Standards: Oser RF Value: Oser Pea>. "actor: Intgral . Jindow Factor ChrTTiif"'- ' mess vin.do PfCS Ch2) TIC Conc- A 1.0CI790, Disabled i.cc: :ao i.c;. Retention Time toins : Relative -:er.tion ".'ire . RT ReEert -ce: Terne Window (mins): Pea< Selection: 7. :::. enabled Disabled Response Type : Response: Polynomial Type: Point o Origin: Pit Weighting: Linear Unies : pea*-to-r * : amplitude: Smoothing; Window sice (scans): pmnri r of smooths: Smocthing method: Join valley threshold: Reduce pV< ruling: Raise ba.i-=ii;.e maximum: Draw ver- .c*'. thrasncld Detect s .Jcrs: Shculder nreshold: Relative -light Absolute icgnt Relative .a; Absolute >rea: 30.00 Disatled 30.CI :.; ;. Disabled j .;;. Disabled 2.3C. Disabled Disabled 9*9* 2 Method Report Method file: La i c Modified: Compound: Printed: C:\MA3SLYMX\scuf0:0H9.pro\HthDB\11059b. Han K3V 0 07:03:59 1999 3: PFDSA (Chii Mon -.3V 08 07:25:54 1 Compound Nan-: Internal ef .; Quantify Trare: Cone, of Standards: Oser RF Value: Osar Peak Factor: Integrate Window Factor: Chromatogram mass window ?r02A (Ch3) Cone. B 1.000000, Disabled 1.0G0S00 2.000 i .o c c o d * Retention Tiste (min. Relative Retention ' RT Reference. Tiae Window (ins): Peak Selection: 3."T:. Enabled . .;0. Disabled Cicr.e] 0.403 Nearest Response Type: Response: :ternal Polynomial Type: Point of Crizm: Pit Weighting ; Axis Tran*crmation Linear Sxclude l/:: ::one Onits: Peak*to-r-**4 amplitude: Smoothing : Window size (scans) Ihiatber of smccths: Smoothing si-*t.`.od: Join valley threshold: Reduce pe <; tailing: Raise b a s - l : m a x i m u m : Draw vert.nl three Detect ah .leers: Shoulder m i eshold : Relative height: Absolute .-.eij.-.t: Relative area: Absolute <rea: E n ab led 2 1 22.C3 ? J . 00 Disabled 30.00 1.!0. Disabled . Disabled 1.00. Disabled :.1:. Disabled Method Report Method lilt: Lest modified; Compound : Printed: C:UliSSLinrt\*:d.':019.proMMtSU10S56. Hon :;ov 08 07:;.-: 53 1999 4: Surr (C14! Mon Nov 08 07:25:54 1999 Compound Mene : Internal Sei. : Quantify Trace: Cone, of Standards: Ueer RF Value : User Peale Factor: integrate Window rector Cbromatog ram mass window: Surr ;Ch4) Fixed l.crOOO, Disabled 1. c::ooo 2. C` : i.c.;:oa Retentior. Time (mina): Relative Jecention Time RT Referer.ee: Time wir.dew (mina): Peale Selection - Bn4bl* ^ Diaadled =I 0*--' Nearest Response Type : Response : Polynomial Type: Point of Origin: Pic Weighting: Axis Trar.stcimacion Linear Exclude 1/7. Unit : peak-to-peak amplitude: Smoothing. Window size (scans): Number of smooths; Smoothing r*tnod: Join vall =-- threshold: Reduce pe < tailing: Raise bas :1ire maximum: Draw vertical threi Detect an: ilders: Shoulder threshold: Relative height; Absolute ..eight: Relative area: Absolute area: 93. lis .ed 33. 1. ! .. Disabled C . . Disabled 2. C1. Disabled 3.3. Disabled Quattro U, #6414E SOUP 020199: FACT Equipment Log 99092 PAGE 1/1 DATE: 11-05-99 ANALYST:mmh STUDY NUMBER: TOXI45 MATRIX: rat sera DESCRIPTION: day 29- dii FACT Method: ETS-8-5.1 Injection volume10 ul. Cycle time: 10 min. Electrode: Z-$pray Mobile Phase: (A12.0 mMNH4CH3C02 (B MeOH TN-A- or stndrd number (A) 99Q85- H -.15------------ IBI TN-A-2997 Prepared (date/by): ( M 10/30/99 sah______ fBl 10/30/99 sah Expires: (A)Q4QQ---------------- (B)_2Q12____ Store atroomtemp? or N Other:_ Guard column: None_________ _____ Part number:jia_______ Lot number: na Analytical column: KeystoneBetasil Size: 2 xSOmm_____________ Type:.18_________ Sphere size: 5 urn---------Partnumber: 055-701-2_______ Lot number: P9E11 Serial number:0591804Z Analytical parameters: Drying gas (L/hrl: 350 ESI nebulizing gas(L/hrl 13 LC Flow rate: 100 ul./min. Back pressure: 65 bar Sheath gas (L/hr)J). HPLC solvent gradient: 10min-10-95 Time (min.l DJLQQ____________ 2)_LQQ_________ 31 5.50_______ 41 7.50__________ 51 8.00_______ %B iM 1M_ 95.0 95.0 10.0 Tuning Method Report M ethod: C : \M ASSLY1DC\SOUP020199.PR 0\A C Q U D B \PF0S3 Printed: Fri Nov 05 1 5 : 3 2 : 0 5 1 9 9 9 Page 1 SOURCE ( E S P - ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. S e t Rdbk 1.60 40 5 0 .2 150 250 1.60 -60 -6 149 249 Pressures Analyser Vacuum Gas Cell Rdbk 5.1e-5 4.le-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set 14.0 14.0 0.9 0.0 4 650 Set Rd] 14.0 14.0 10 2.0 0.0 40 0 650 42 40 45 mtioa. c,\aM,vxx\toar70U*.no\tcaaa*\i.iima-m*-fo^-> L est M odified: F ri O ct IS 10*35*03 19** m a te d : F r i Mow 0 5 1 5 :3 1 * 3 * 1 * __________ S o lv e n t D elay ( a ln a ) : 0 .0 0 F uaetlen : 1 IBM o f 1 m o m F a i r ( * * - ) I n te r C hannel D elay ( Seca ) : Span ( D altons ) : S ta r t Tuae ( M ins ) : End T M ( M ins ) : R epeats : C hannel P a re n t D aughter 1 413.00 149.00 0 .0 3 0.00 0.00 10.00 1 D w ell (S ec s) C o ll E n ergy (eV) 0.30 30 Cone ( V ) 15 F unction : 2 MtM o f 1 M ess F a i r ) I n t e r C h a n n e l D e la y ( S e c s ) Span ( D altons ) : S ta rt T iM ( K ins ) : End Time ( K in s ) : R epeats : C hannel P a re n t D aughter 0 .0 3 0.00 0.00 10.00 1 D w ell (S ec s) C o ll Saergy (eV) 1 499.00 99.00 0.30 45 Cono ( V ) SO F unction : 3 mrm o f 1 M esa F a i r ( B E F- ) I n t e r C hannel D elay { S ecs ) : Span { D altons ) : S ta r t T iM { M ins ) : End T iM ( K ins ) : R epeats : C hannel P are n t D aughter 0 .0 3 0 .0 0 0.00 1 0 .0 0 1 D w ell (secs) C o ll Energy (eV) 1 499.00 7 8 .0 0 0.30 45 Cone ( V SO F unction : 4 MM o f 1 M ess F a i r ( B>F~ ) I n t e r C h a n n e l D e la y i[ S e c s ) : Span ( D altons ) : S ta r t T iM ( K ins ) ; End T iM { M ins ) : R epeats : C hannel P a re n t D aughter 0 .0 3 0.00 0.00 1 0 .0 0 1 D w ell (S ec s) C o ll to a rg y (eV) 1 427.00 80.00 0 .3 0 40 Cene { V SO Page 1 Masslynx - Sample List Sample Ust: C:\MASSLYNX\soup020199.pro\SampleDB\110599b.SPL Printed: Fri Nov 05 15:26:20 1999 Page 1 Page Position: (1,1) File Name File Text MS Rle Inlet File 1 110599028 MeOH Blank 2 110599029 MeOH Blank 3 110599030 MeOH Blank _____ 4 110599031 TOX145-RBS11039-H2O Blk-9, ext. 11/3/99 MCH 5 110599032 TOX145-RBS11039-Sera Blk-9, ext. 11/3/99 MCH 6 110599033 TOX145-RTS11039-Sera Blk-9, ext. 11/3/99 MCH 7 110599034 TOX145-RBS11039-5ppb-9, ext. 11/3/99 MCH 8 110599035 TOX145-RBS11039-10ppb-9, ext. 11/3/99 MCH 9 110599036 TOX145-RBS11039-25ppb-9, ext. 11/3/99 MCH 10 110599037 TOX145-RBS11039-50ppb-9, exL 11/3/99 MCH 11 110599038 TOX145-RBS11039-100ppb-9, ext. 11/3/99 MCH 12 110599039 TOX145-RBS11039-250ppb-9, ext. 11/3/99 MCH 13 110599040 TO X145-RBS11039-500ppb-9, ext. 11/3/99 MCH 14 110599041 TOX145-RBS11039-750ppb-9, exL 11/3/99 MCH 15 110599042 TOX145-RBS11039-1000ppb-9, ext. 11/3/99 MCH 16 110599043 MeOH Blank 17 110599044 TOX145-RTS-9R03255M-5mg/kg-Day29, D:10 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 10min-10-95 10min-10-95 10min-10-95 10mln-10-95 10min-10-95 10min-10-95 10min-10-95 10min-10-95 10min-10-95 10nnin-10-95 10mln-10-95 10mln-10-95 10min-10-95 10min-10-95 10min-10-95 10min-10-95 18 110599045 TOX145-RTS-9R03256M-5mg/kg-Day29, D:10 19 110599046 TOX145-RTS-9R03257M-5mfl/kg-Day29, D:10 20 110599047 TOX145-RTS-9R03258M-5mg/kg-Day29, D:10 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 10MIN-PFOS-POAA-PFOSA-IS 10mln-10-95 21 110599048 TOX145-RTS-9R03259M-5mg/kg-Day29, D:10 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 22 23 24 110599049 TOX145-RBS11039-250ppb-CCV9, ext. 11/3/99 MCH 110599050 MeOH Blank 110599051 TOX145-RBS11039-H2O Blk-9, ext. 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 10mln-10-95 10min-10-95 25 110599052 TOX145-RBS11039-Sera Blk-9, ext. 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 26 110599053 TOX145-RTS11039-Sera Blk-9, ext. 11/3/99 MCH 27 110599054 TOX145-RBS11039-5ppb-9, ext. 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 28 110599055 TOX145-RBS11039-10ppb-9, ext. 11/3/99 MCH 29 110599056 TOX145-RBS11039-25ppb-9, ext. 11/3/99 MCH 30 110599057 TOX145-RBS11039-50ppb-9, ext. 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 10MIN-PFOS-POAA-PFOSA-IS 10mln-10-95 31 110599058 TOX145-RBS11039-100ppb-9, ext. 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 32 110599059 TOX145-RBS11039-250ppb-9, ext. 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 33 110599060 TOX145-RBS11039-500ppb-9, ext. 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 34 110599061 TOX145-RBS11039-750ppb-9, ext. 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 35 110599062 TOX145-RBS11039- 1000ppb-9, ext. 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10m in-10-95 FACT: DA TA REVIEW SUMMARY FORM f Hate Data Analyst. ST*aSj* ------------------------------------------------------------ ' "" ~Trri //< -------------------- ------ Matnx/Timcpoints: f>/,a j 1j r n i l . . . , rjH frar ffaa-c J-S------ 's/--u <h-rf/ lo / ie - ----------------- --------------- ---------------------- Data Review Sign-OfT Analyst Review Name / Date: i. I3/ / f / f ' f ________________________ _ L - ^ r - ^ s r , M , s / A-* t f / t f / g / t '1 Quality Assurance Review Set-up Analysis Date/Analyst: Instrument: /*//* rrr-- 1* --------------------------- -------------------- Data Entry:_______ L A C I d / ^ / ( ---------------------- Comments /Justifications: ________ __________ ___________ Analyte: ToAA r ,u ,> & Z ___________ Acceotable Linear Range: A /, rivi*. OPatlLL-----S ee I.OO: AM Extraction Blank: fJ/A RA2: //4 Matrite Blank: ^ Calibration Checks: hlA M S/MSD:________ Data Status: ftfc-friAr. ip<3|n l 6 rr *Lm-L+ >4^^ d-V-*- ^ L ^ dL s n L J J 0 P<>AA dnJ*- &* m t K J i s * J i f i s c l / y g * -- L > r > 4 I c __ V iR f i f .*?--------------- Analyte: ?)cbS --w Acceptable Linear Range: A 3 ^-7^ ^ ---------------- LOQ: _______ Extracted Blank: lets 4l**- t* A L /r a a < t, 4 i t j j d t ' d t l 4 - --------- ilAA^S *j,L "&* fU-i'U<r------^ 5.)as s lr y ix .1 **-- -iL.-- RA2: Q . m t ' f t Calibration Checks: 0K ~ Matrix Blank: esc JUo.il. Lo<X -Pran^. / i 7 ,7 ^ ) /' M S/M SD :. Data Status ^ rr bvU /til vJYtliAfenJ HCizU. Analyte: ?FSA CCHz'y ( ) Acceptable Linear Range: i~l */jj>L ----~~? U j .ttd l- LOQ: h . boit Extracted Blank: J s ^ J iiiJ d A r 2: 6 . ifa `tS '9 <f _______ Matrix Blank: / t c L>&. Calibration Checks: OK- -- ->-- ~ 3 ^ /o MS/MSD: Data Satus: EnW ftd T UC, lo b liii- "4 4 ,1 t t z o t j - r d o I ^ J k t L ^ v '- e . ------ (s s 4 l-i Ld Q . Sa n y a s tu r f J J u-J-i^nS--- Q**- <rf J-Lfr Cot&*'aL-- / S u t bhL* v e U l U -- J jL ^ t --- "7%*- -- sL > S o r ^ i u ' r j o L ^ k ' ____ ~ ~ - ^ S T U t ^ \ --1ZIJT^-*---------- s J / 2 U * * i Cj l V\>+ J p to fa t h u * r c . -------------- h t (.ut*- ' mj J i'J tJ f t l . --------- J k i di*. KnftA . K fttJLVtX. ?)0^ J u 3* ***- P A A d i k e * * * ' 1 * * * * " ') * n , t Q gvvun s t i f t e M lo iS tfO il 5 0 u a^ c4 c u r r y -c v tV k k tO W M f) / ' Dale: Data Analyst: KACT Study#: Mn /ti J*S 7> H tr Matnx/Timepointa: ^ Sample List: Set-up Analysis Date/Analyst: frfrrfil FACT: DATA REVIEW SUMMARY FORM ^ Data Review Sign-OfT Analyst Review Name / Date: 3-S A / / r / f y _________ f - L m ts, fatilr J * f i f /ah f Technical Review Name / Date:_____ , L r 4-to pfl<yg, Quality Assurance Review rd Name / Date:_____________ 1 p 2- LA- 1% < / m Data Entry: _ ul io /iiK q oup 020199: Q u a n tifie d and p rin te d by id* 10/19/99 U uU ukJU U H H SwW HUlHilSvW 3&&3&3B3? H H iWn wW uWa a H 5 UtOOt StOMOO 3 33333???? !3 MMMMwUvI Vm gai a O OOOUU4 UMMM 333333333333 %1 M W H M M N ft. ^ ^ i f U U Ul ? ?5???3 HHHW MW sj . Ul 353335 M M HW aHW HW M M M W HHHa M M WUI M U K Ut ?3S??33?3533S3S??5 it > et -4 o m1mM j te wo u> *4 -4 <e o *> o w o o l-M M M H H O 01 U <4 < 4 iM U 4 U M Ut O K I O M u a u u iM tit u> et o Oo oO Hu kO Up aO Me Oo aM Oo MH OOI M Uk^uUo>u4 ii Oo Oo tt n r t oup 02019t: Q u a n tifie d and p ria ta d by ia a 10/19/99 I S5SSSSS533SSSSS5SS33SSSSSS3SS3SS3SSSSSSSS3SS3SS5SSSSSSSS55SS5B j E ssS srsS a sssssS ssS ssssK K S sS S c sH sS ssstssssa sa ssK sssa sa a sstsl gm S Sgg*i& m im sm m & K *m m 5m & B S& ti9im S g& m SS8gS5m 3 5 5BsSasM- . t s 3 s L s . s s l I . S o S s s s B 3 . s . ! L . B s - - - . . s c s S s s M- - - -- J b sa sb E isg S S sssg sssssg sg c s-ssc g g a sg g d sg g g g g a sssssg g g g g g ? J ,, . i l g a ? PP* g 88 n- p- \r o $ ? 2** 4% P fr P g licg r Br Prr?--- ,* Kg D Pr -- cc.-isg f en Ut >? -*-* P - ?= rr iL r^ Q u u C if y Ccwpnnnil S u n u iy K a p e rt _ TOXI4 5 - r a t l i v e r , d a y 1 4 , c o n t r o l a n d d e a # - a t 1 0 /1 3 /9 9 S e g a le L i t : C : \H A S8LTX X \aoup-rata .p r e \ i^ la n B \1 0 1 5 9 9 a L a s t o d i f i a d : Meo O c t 1 0 4 : 4 2 : 0 1 V M . . MatKod : C : \us8L T fioi\aoup-rata .pro\M efchB \101399a L a s t M d l f i a d : Men O c t 1 0 4 : 4 1 : 2 1 190* Jo b Coda: P rin te d : Men O c t 1 0 9 :3 0 :0 2 1999 CcMpouad 2: prosa (0x3 ) 0 Nana 1 101599001 2 101599002 3 101599003 4 101599004 5 101599005 6 101599006 7 101599007 8 101599008 9 101599009 10 101599010 11 101599011 12 101599012 13 101599013 14 101599014 15 101599015 16 101599016 17 101599017 18 10159901B 19 101599019 20 101S99020 21 101599021 22 101599022 23 101599023 24 101599024 25 101599Q2S 26 101599026 27 101599027 23 101599028 29 101599029 30 101599030 31 101599031 32 101599032 13 101599033 34 101599034 35 101599035 36 101599036 37 101599037 38 101599038 39 101599039 40 101599040 41 101599041 42 101599042 43 101599043 44 101599044 45 101599045 46 101599046 47 101599047 48 101599048 49 101599049 50 101599050 51 101599051 52 101599052 53 101S990S3 54 10 15990S4 55 101599055 56 101S99056 57 101599057 58 101599058 59 101599059 60 101599060 61 101599061 62 101599062 63 101599063 4 101599064 S am plelist Tant MeOH B la n k HOK B la n k MeOH B la n k T0X14S, RBL10139-K2O B la n k -1 1 , SO TOX145, TOX145, TOX145, TOX145. T0X145. TOX145. T0X14S. RBL1013 9 - L i v e r B l a n k - 1 1 . R 8 L 1 0 1 3 9 - 5 p p b - l l . SSB R B L 10139-10ppb-ll. S O R S l.l0139-25ppb-ll. S O R B L10139-50ppb-ll, S O R B L10139-100ppb-ll. S O R B 110139-2S0ppb-ll, S O SO TOX145. R B L 1 0 1 3 9 -5 0 0 p p b -U . S O TOX145. R B L 1 0 1 3 9 -7 5 0 p p b -ll. S O TOX145, R B L 10139-1000ppb~ll. S O MeOH B la n k TQX145. RTL-9R03230M. D y l. C o n tr o l - S O 1 0 /1 3 /9 TOX145, RTL-9R03231K. D y l. C o n tr o l- S O 1 0 /1 3 /9 TOX145. RTL-9R03232K. D y l. C o n tr o l- S O 1 0 /1 3 /9 9 TOX145. RT.-9RQ3233K. D y l, C o n tr o l - S D 1 0 /1 3 /9 9 T0X14S. RTL-9R03234JI. D y l. C o n tr o l- S O 1 0 /1 3 /9 9 TOX145. R B L 10139-250ppb-C C V -ll-l. S O MeOH B la n k TOX145. RTL-9R03235M. Dy4. C o n tr o l - S O I O '1* ' " T0X14S. RTL-9R03236M. Dy4. C o n tr o l - S O 1 0 /1 3 /9 9 TOX145. TOX145. T0X14S. T0X14S. RTL-9R03237M, D y4, C o n tr o l - S O RTL-9R03238M. Dy4. C o n tr o l- S O RTL-9R3239M. Dy4. C o n tr o l - S O R B L10139-250ppb-C C V -ll-2. S O 1 0 /1 3 /9 9 1 0 /1 3 /9 9 MeOH B la n k T0X145. 9R03230M, D y l. C o n tro l-2 5 0 p b -K S -H TOX145. 9R03230M. D y l. C o n tro l-2 5 0 p b -M S D -ll TOX145, 9R03235H. Dy4. C o n tro l-2 5 0 p b -K S -1 2 T0X14S, 9R03235M. Dy4. C ontrol-250pb-M S D -12 TOX145. RTL-9R03245M. D y l. SnQ /kQ - S O 1 0 /1 3 /9 9 TOX145. R B L l0 1 3 9 -2 5 0 p p b -C C V -ll-3 . S O MeOH B la n k TOX145. R B L 10139-250ppb-C C V -ll-3. S D MeOH B la n k T0X14S. RT1-9R03246K. D yl. 5 n g /k fl- S O 1 0 /1 3 /9 9 TOX145, TOX145. TOX145. T0X14S. TOX145, RTL-9R03247H. D y l. S a Q /* 9 ~ S O RTL-9R03248M, D y l. 5 g /k g - S O RTL-9R03249M, D y l. 5 /k g - S O RTL-9R032S0M, Dy4. 5 Q /k g - S O RBL10139-250ppb-C CV -ll-4, S O 1 0 /1 3 /9 9 1 0 /1 3 /9 9 1 0 /1 3 /9 9 1 0 /1 3 /9 9 MeOH B la n k TOX145, R B L 10139-250ppb-C C V -ll-4, S O MeOH B la n k TOXI4 5 , RTL-9R03251M , Dy4 , S n g /k g - S O T0X14S, RTL-9R03252M. Dy4. S n g /k g - S O T0X14S. RTL-9R032S3M. Dy4. 5 a ff/k g - S O TOX145. RTL-9R03254M. Dy4. 5 n g /k g - S O TOX145, R B L 10139-250ppb-C C V -ll-4. S O 1 0 /1 3 /9 9 1 0 /1 3 /9 9 1 0 /1 3 /9 9 1 0 /1 3 /9 9 MeOH B la n k T0X14S, R BL10139-250ppb-C C V -ll-4. MeOH B la n k T0X 14S, R B L 1 0 1 3 9 - S p p b - ll. SSB TOX145. R B L 1 0 1 3 9 - 1 0 p p b -ll, SSB T0X14S, R B L10139-25ppb-ll, S O T0X 14S. R B U 0 1 3 9 - 5 0 p p b - l l . SSB TOX145, R B L 10139-10O ppb-ll. S O TOX145. R B L 1 0 1 3 9 - 2 S 0 p p b - ll. SSB TOX145, R B L 1 0 1 3 9 -5 0 0 p p b -ll. S O T0X14S. R B L10139-750ppb-ll. S O T0X14S. R B L l0139-1000ppb-ll. S O S tan d ard S tandard S tandard S tandard S tandard S tandard S tandard S tandard S tandard OC oc oc OC oc oc oc oc S tan d ard S tandard S tandard S tandard S tandard S tandard S tan d ard S tandard S tandard 6 .1 4 12.40 31.00 62.00 1 2 4 .0 0 3 0 7 .0 0 614.00 9 2 1 .0 0 1 2 2 8 .0 0 307.00 3 0 7 .0 0 307.00 307.00 307.00 307.00 3 0 7 .0 0 3 0 7 .0 0 6 .1 4 12.40 31.00 62.00 124.00 3 0 7 .0 0 6 1 4 .0 0 9 2 1 .0 0 1 2 2 8 .0 0 7 .8 1 0 7 .8 2 6 7 .8 3 9 7 .7 9 6 7 .8 0 7 7 .7 6 6 7 .7 8 3 7 .8 0 5 7 .7 9 2 7 .8 0 8 7.814 7 .8 0 7 7 .8 1 3 7 .8 0 8 7 .8 4 8 7 .8 5 2 7 .8 3 3 7 .8 3 5 7.B 13 7 .8 1 3 7 .1 1 3 7 .8 7 4 7 .8 2 4 7 .8 3 3 7 .8 0 7 7 .8 5 7 7 .8 3 3 7 .8 0 9 7.855 7 .8 1 3 7 .8 1 3 7 .8 1 4 7.811 7 .8 0 7 7 .8 1 3 7 .8 5 8 7 .8 0 7 7 .8 5 7 7 .8 0 6 7 .8 0 6 7 .8 1 3 7 .8 1 4 7 .8 5 7 7 .7 9 2 7 .8 8 1 7 .8 1 0 7 .8 7 9 7.816 7.806 7.812 7 .7 9 0 7.804 7 .8 8 0 7 .8 1 0 7 .8 7 9 7 .8 3 6 7 .7 9 1 7 .7 9 0 7 .7 8 9 7 .8 1 3 7 .8 1 3 7 .7 9 2 7 .8 1 2 7 .8 1 0 p*e 3 A rea P lace 177 bd 339 bb 178 MH 145 MM 159 MM 321 MMX 522 MM 1469 MM 2173 MM 4263 MM 10398 MM 2 0 565 MM 26902 MMX 35703 MMX 166 MM 147 MM 115 M( 127 MM 140 MM 127 MM 8203 MM 105 MM 2 7 7 MM 147 XX 77671 db 352 KM 183 MM 8271 MM 123 MM 10526 MM 9524 MM 7882 MM 7389 NK 147648 db 8382 MM 158 MM 7 9 4 1 KM 138 MM 176413 dd 153273 dd 156909 bb 160875 db 932 MM 7589 MM 202 KM 7441 MM 172 MM 66310 bb 73496 dd 68288 dd 79669 bb 7292 MM 211. MM 74801 KM 1481 KM 367 MMX 551 MM 1467 MM 2 2 0 5 MM 4136 MM 1 0 131 MM 2 0 6 5 9 MM 25247 MO 35305 MMX Cooc. tfivr 0.00 4 .2 5 0.00 0.00 0.00 3.70 -40 9.78 -21 3.38 24 59.64 -4 1 2 2 .7 9 -1 3 0 8 .1 6 0 6 1 5 .3 0 0 0 6 .7 7 -12 1072.65 -13 0.00 0.00 0.00 0 .0 0 0 .0 0 0 .0 0 241.81 -21 0 .0 0 lAC io o '" -Mud 4 .6 2 0 .0 0 243.87 -21 0.00 312.02 2 8 1 .7 2 2 3 2 .1 3 217.22 4 54.76" W t t d 247.24 -19 0.00 233.92 -24 0.00 323.8 1 \ 1 a I'.ido l l v * ww I.|dd Liu. 854.39r> 22.16*^ 223.26 -27 0.11 218.79 -29 0.00 9 9 7 .3 5 ^ 21*.16 l l W i q 057.11 < 40 0 .9 8 J 214.29 -30 0 .3 8 219.99 -28 0.00 5.07 -17 10.64 -14 3 8 .3 3 24 60.61 -2 118.95 -4 300.07 -2 6 1 8 .1 6 1 756.78 -18 !'IDo di)ui*y ! IDO d iL lic v , u lo f Ondi Soup 020199: Quantified and printed by laa 10/18/99 s n v a v io o o o o o * O O O O H H H ^H rtO 9^00 oc Hr rOfilTiVinvntiAdM 11f*t* >oo o o o o o o * 2 2 2 S <* 2 O oI o on o O O O O O O O O O 4 * *> *4 O * * O o o > O O r* ri -4 H O O O c aaaasaaaaaa aaaaaa aaaaaa aaaaaa a aaaaaa aaaaaaaaa aaaaaaaaa g M AcmnocoHHh n n w m #i 4 r- J l S 2 2 i 2 S a o S a n m 9 i9ihM > O N O O i ? SSS5S5SSSS5 SSP3S5 SS3333 SSSSSS S SSSSSS 3 3 3 333 3 333333333 4 HHHHHHHHHH HHHHHH H f i H H H H r4 H H H H f l H - <3'- nt Si cJ 3 H r H n 9 i i n 9 i a 4 a i a (i M n n 4 2 2 2 2 E 2 a oais 2 5 P 3 2 ? 2 2222222o *3 B SSSSSSSSSSS SSSSSS SSSSSS SSSSSS S S S o o o o o-oooooo. o o o o o o o o o g f ^ r. ' r ! r - . r ^ r 'r - r - r r 'r * r- r- r- r* r- i-* t- r r- r- r- f- r r t* r r r* f r- r- r- r* r* f- r - r - r - r - r - r - f t - f * r r* r- r ,'j. _o o ~~ozt Il 3 l 8 a lim i 88 r> <3 r a 1:1: i H 4 Hs H^ I k n CkH un ^ O />0 8:8= t) **>1> \\\ti\I i s33i it3i2l3i* jS il 3313 3 o o o o o e o o o ooooo B"a asaaS IH N H H U W H M -Si 8^O > I ri I I I l i i xt J A J a 1ls afataao oaa aao aaooao iOOlAOKIO BSBBB,, HHHriH SUb &Ud 8lai SUaSUd-n-I 3U0 U0 U0U0-I ri ri ri ri ri O SSSSS& ias's's's i>fnoi rnoionn nno na BSBBB. i lg 4444-B Bassa HUVUAMH aosar, (A (A VI I M (A SSS*fH r4 H H H oNiNonHomrionaBii 4 OOOOS M M + iSSifUJiiiJSiHSS.8i u-gaug-u58ouVg^-S.BBi 5>i8 ;B B. . . - j j rOi rO-l Or i Or4 Of 'rii & SS5S ? im i? ? SSSi a 3S X...X.....X...*......X... &O t - a Oa q>o itn . fX.i nX. .X* Oian nno nnaimnqninrorn}noi **.i4 onjoi_ftIjif)_l| S U U UU H H M IM NM MHH IMM . . , r i H H ri ri gla ooa aadaoaSoaSoa Soa ooS 8 3MOOMOMO >0000000 io o o o o JJJ JJJ J J a rJ J . :ssse SK etgieK k*K B C K ***S o o o o J a a : ei oc k c i aaaaaa 5"'a;cess*ce*m5*a j ja a a a a a a i( i B d d d d a i iiiiiiliiiiiiliiiiilllslliiiisiiiiiisisiiiiiisisiiiiisiaiiiiiiBii Sooooooooooooooooooooooooo ISrtoroiroiHoHoHorolHoHoHoroiroiHo roiroiHo rotHo Ho Ho Ho Ho oHoHbHbrlbHbrfbHbribHoriortcr " -^ r ^r n 4 i f l i h > l f H0 r' ii rHii <4 4iiinHir) ir H' H0H'(0 1" Ni Mr iNnN-f*1l f lNNl Nh i0 40 f' 0>'ri tr (i i42r' >000000000 3o o o o o c a o o o o o o o o o o c c 50 2b U o Q. goup 020199: Q u a tlil 4 ad p rln r* d by l* a 10/11/99 *S iofu h ? J - / / / / * 1 ioup 0301: Quaatltlad ind printed toy la* I0/lt/99 a* 2 up 020199 : Qu*ntlXl ts printed by i u 10/19/99 3 oup 020199; Quantici! and printed by laa 10/19/99 X >0CX' Vag* 4 oup 020199 t Ou*atlld Ad printed toy !* 10/19/99 M athod R aport M ethod f i l a : Laat n odifind: Compound: C : \KASSLYNX\ a o u p - r a t a . p ro \M a th D B \1 0 1 S 9 9 a .m d b Mon O c t 18 0 6 : 4 1 : 2 1 1999 1 : POAA (C h i) MOD OCt 18 0 7 : 4 6 : 5 1 1999 Compound Mama: X ntam al Raf.: Q u antify T raa: Cone, o f S tandarda Q a a r RF V a lu a : O aar P<k F a c to r: X n ta g r a ta Window f a c t o r : C hrom atogram m aaa window: R a ta n tio n Tima <*ina>: R a la tiv a R a ta n tio n Tima: RT R a f a r a n e a : Tim a Window (m ina) : Panic S a l a c ti o n : Raaponaa Typa: Raaponaa: P olynom ial Typa: P o in t o f O rig in : F it W aighting: A xia T ra n n fo n aa tio n : POAA (C h i) 1.000000, 1 .0 0 0 0 0 0 2.000 l.OOOODa D iaahlad 7.129. 0.000, (N ona] 0 .3 5 6 S n a b la d D iaahlad N aarast E xtarnal A rana L inaar K xcluda 1 /z Nona U nit: Paak-to~paak aavlituda: Sm oothing: Window a i s a (a c a n a ) Numbar o f am ootha: Sm oothing m ethod: Jo in v a lle y th raahold: Raduca peak ta ilin g : R n ia a b a a a l i n e ma ximum Draw v a r t i c a l th r a a h o ld : D atact ah o u ld a ra : S houldar th ra a h o ld : R alativ a b aig h t: A baoluta h a ig h t: R alativa araa: A baoluta a ra a : 66 E n a b la d 2 1 3 0 .0 0 200.00 5 .0 0 9 0 .0 0 D iaahlad 3 0 .0 0 1 .5 0 , D iaahlad 0 .0 0 , D iaahlad 2 .0 0 . D iaahlad 0 .0 0 , D iaahlad Xn-s i * / i s h f J,- //V f Pag# 1 5 o p OZ a /7 1 --- f M ethod R eport M ethod f i l e : L is t m odified: Compound: P rin ted : C :\H aSSL Y M C \soup-rat*.pro\H ethD B U 01599e.m db Mon O c t 18 0 4 :4 1 x 2 1 1999 2> PPOS (Ch2! Mon O c t 18 0 7 x 4 4 :5 1 1999 ____________ C p o u n d Name: in te rn a l R ei-s Q u antify T race: Cone, o f Stender!*: O s e r RP V e lu e : O ser Peek F acto r: I n t e g r a t e Window F a c to r : C hrom atogram a a s i window: p ro s (Ch2) (Mone) TIC Cene. B 1 .000000. 1.000000 2.000 1 . 00000a D isabled R eten tio n T ins ( s in s ) : R e la tiv e R eten tio n Tine: RT R e f e r e n c e : Tim e Window ( m in s ) : peak S electio n : 7.213. E nabled 0.000. D isabled (Mona) 0.400 n e a re st Response Type: Response : P olynom ial Type: P o in t o f O rig in : F it W eighting: Axis Transformation: E xternal areas tannar E xclude 1/X Hone Units : P eak-to-peak am plitude : Sm oothing: Window s i z e (s c a n s ) Mumber o f sm o o th s: Sm oothing m ethod: jo in v a lle y th resh o ld : Reduce peak ta ilin g : R a i s e b a s e l i n e ma inimi 66 E nabled 2 1 30.00 200.00 S .0 0 Draw v e r t i c a l th r e s h o ld : D etect sh o u ld ers: S houlder th re sh o ld : R elativ e h eig h t: absolute height: R elative area: ab so lu te area: 90.00 D isabled 30.00 1.5 0 . D isab led 0 .0 0 . D isabled 2 .0 0 . D isabled 0.00. D isabled oi> ni 2 M ethod R eport M ethod f i l e : L ast M odified: Cos^ound: P rin ted : C :\M A SSL Y N X \soup-rata.pro\llethD B \101S99a.m db lu n O c t 11 0 6 :4 1 :2 1 1999 3: ffOSA (C h3> Hon OCt 18 0 7 :4 6 :5 1 1999 C eev o u n d Marne: in tern a l Ref.: O uantify T race; Cone, o f S tandard: U s e r RF V a lu e : U ser Peak F acto r: i n t e g r a t e Window F a c to r : C hrom atogram m ass window: p ro s * (Ch3) (None] TIC Cone. C 1.000000. 1 .0 0 0 0 0 0 2.000 l.OOOODa D isabled R e te n tio n T i e (m ina) : R e la tiv e R eten tio n T ie: RT R e r e n c a : T in a Window (m in a ): Peak S e le c tio n : Rasponee Type: R esponso: P olyncaal Type: P o in t o f O rig in : P it W eighting: A xis T ran sfo rm atio n : 7.797, 0.000. [None] 0 .6 7 9 E n ab le d D isabled N earest E xternal A reas L inear E xclude 1/X None U nits: P eak-to-peak asip litu d a : 80 Sm oothing: Window s i s e (s c a n s ) Nunber o f sm ooths: Sm oothing m ethod: jo in v alley th resh o ld : Reduce peak ta ilin g : R a i s e b a s e l i n e ma v i m na Draw v e r t i c a l th re s h o ld : D etect sh o u ld ers: S houlder th re sh o ld : R elative h eig h t: A bsolute h e ig h t: R elative area: A bsolute area: 3 0 .0 0 200.00 5 .0 0 9 0 .0 0 D isabled 30.00 1.S 0. 0.00, 2.00. 0.00. D isabled D isabled D isabled D isabled PQB 3 "? * -s / R eport M ethod f i l e : L ast M odified: Compound: P rin ted : C :\K A SSLY H X \soup-rata.pro\M ethD R \101S99a.m db Moa O c t IB 0 6 : 4 1 : 2 1 l * * 9 IS <Ch4) NOB OCt 18 0 7 : 4 6 : 5 1 1999 Compound NasM : In tern al Ref.: Q u antify T rac: C oac. o f S tandard'. U s e r RF V a lu : Oar Peek P acto r: I n t g r t Window F a c to r: C hrom atogram m ass window: IS (Ch4) I Moa] TIC F in d 1.000000, 1.000000 2.000 l.OOOODa D isabled R etention T i (nine): R e la tiv e R eten tio n Tuse: RT R e f e r e n c e ; T in e Window ( a l a s ) : Peak S elec tio n : 7 .157, 0 .0 0 0 . (N o n } 0.411 B nabled D isabled H aarest R esponsi Typ: R esponse: P olynom ial Type: P o in t o f O rigin: F it w eig h tin g : A xis T ran sfo rm atio n : E x ternal A reas L inear E xclude 1/X Hone U nita: Peak-jto-peek s o litu d e Sm oothing: Window a i s e {scans} Humber o f sm ooths: Sm oothing m ethod: Jo in v alley threshold: Reduce peak ta ilin g : R a is e b a s e l i n e maximum: Draw v e r t i c a l th re s h o ld : D etect sh o u ld ers: S houlder th re sh o ld : R elativ e h eig h t: A bsolute h e ig h t: R elativ e area: A bsolute area: 67 E nabled 2 20.00 200.00 5 .0 0 90.00 D isabled 10.00 1.5 0 . D isab led 0.0 0 , D isab led 2 .0 0 , D isabled 0.00, D isabled Pag 4 5 Quattro EL, #6414E SOUP 020199: FACT Equipment Log 99092 PAGE 1/1 DATE: 10/15/99 A N A L Y S T iiss , S T U D Y NTTMBFRr T O X 145 M A T R IX : p it liv g n D E SC R IP T IO N : d W 1&4 FACT Method: ET S-8-7.0 Injection volume: IQ uL M obe Phase: C y c le tim c:J Q m in, E lectrode: Z - S p lll!------------ n mM NH4CH3CQ2 (B )-M sQ H ---------- T N -A - or stndrd num ber (A ) 9 9 0 8 5 -1 0 -5 ---------------- Prepared (date/by): (A ) 1 0 /1 0 /9 9 ,^ ------------- (B) TN-A-2378-- (B ) 1 0 /1 0 /9 9 &ah. Expires: (A -) 0 4 / 0 0 ________________ Store at room tem p? Y] or N O ther:. (B)_2Q 1S------------ G uard colum n: None Part number: na________ Lot number: na A n a ly tic a l rnh tm n : K eyston e R e t a s i l _______________________________________ Sire: 2 x 5 0 mm_______________ ___ T yp e:_18--------------------- Sphere size:_Lum _ Part number: 055-701-2 Lot number: P9E11 S erial nnmher:0 5 9 1804Z A nalytical param eters: D rying gas ( L / h r ) : J 5 0 _ _ E S I n eb u lizin g gas (L /h r)J 3 ------ Sheath g a s (L /h r)Jl LC F low rate: 3 0 0 uL/m in. B ack pressure: 65 -- HPLC solvent gradient: 10min-10-95 Time (m in.l 110 .0 0 __________ 21 1.00_______________ 3 )-L 5 Q _______________ 4 1 7 .5 0 __________ 5 1 8.00_______________ 1Q.-.L 1Q.0 -210 21S_ 1M _ Tuning Method Report Method: C :\ M A S SLYNXXSOUP-RATS.PR0\ACQUDB\PF0S3 Printed Fri O c t 1 5 1 1 : 4 2 : 3 2 1 9 9 9 Page 1 MS SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. MS2 Set Rdbk 3.00 40 5 0 .2 150 250 3.00 -41 -6 153 250 Pressures Analyser Vacuum Gas Cell Rdbk 6.6e-5 4.le-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set Rdbk 14.0 14.0 0.9 0 .0 4 650 3 Set Rdbk 14.0 14.0 10 2.0 0.0 40 0 650 7 38 -0 f n i m 4**g Wthnil Upset c,^MMMMvm \ m m - t x n . T K \ u x r a m \ i i u B - w w < - w c u - w n u . - z t r r l O ct 13 lltS S iO S 1 I n t a r C hannel D elay ( S acs ) Span ( D altons ) : S ta r t T in e ( M ins } : Snd T ina ( M ins ) : l * P * * t *C h:a n n e l P a r e n t D a u g h te r 411.00 169.00 0 .0 1 0.00 0.00 10.00 lu a ll (S acs) c a ll coax Emanme r gwyy (eV) 0 .1 0 30 Cons ( V ) 15 F unction > 2 M o f 1 Mass F a ir ( U P - ) l a t e r C hannal D aisy ( S acs ) : Span ( D altons ) : S ta r t T in a ( M ins ) * n A T in a ( M ins ) s 0 .0 3 J*J ?1!L 1 0 .0 0 `' " '" ' i f c l n n . l . r o o t D ouB O tor i ~ l l <*-=> <==" ' " r o y , * V> =" " < v 1 499.00 99.00 0.30 45 60 F unction l of 1 n i l p air ( * > Intar Channal Dalay ( Sacs ) : Spa n { Daltons ): Start Tina ( Mins > : *nd Tina ( Kins ) : 0.03 0.00 0.00 10.00 " `" " ihinn.l .root D.iht.r D ~ H (Soc.) Col l noray (.V) 498.00 78.00 0.30 45 60 w m o f 1 M ass F a ir ( BSP- ) I n ta r C hannel D alay ( S acs ) : Span < D altons ) : S t a r t T in a ( M ins ) Snd T in a ( M ins ) : C tanool p .r .o t D .u o h t.r 0 .0 3 0.00 0.00 10.00 1 D oll < S .I C o ll tt.rg y (.V ! Cone ( V ) 427.00 80.00 M ethod R e p o rt Method rile: Last Modified: Printed: C:\MXflSLYHX\arOUP-IUlTS.PRO\ACaUDB\10aln-10-95 rriday, October 15, 1999 1143*04 Friday, October 15: 1999 lli43:13 BP1100 LC Pun Initial conditions Solvents M B% C% D% Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 90.0 10.0 0 .0 0 .0 0.300 10.0 0 400 30.0 30.0 HP1100 LC Pusqp Oradient Timetable The gradient Timetable contains 5 entries which are Time 0.00 1.00 5.50 7.50 8.00 A% 90.0 90.0 5.0 5.0 90.0 B% 10.0 10.0 95.0 95.0 10.0 C% 0.0 0.0 0.0 0.0 0.0 D% 0 .0 0 .0 0 .0 0 .0 0 .0 Flow 0.300 0.300 0.300 0.300 0.300 HP1100 lc Punv Maternal Meant Timetable The Timetable contains 3 entries which are : Time Initial 0.00 0.10 Column Switch Contactl Off Off Off On Off Off Contact2 Off On Off Contact3 Off Off Off Contact4 Off On Off HP1100 Autoaaaplar Initial Condition Draw Speed Eject Speed (pl/min) Draw Position (mm) Stop Time (mins) Injection Volume(pi) Vial Number 200.0 200 0.00 9.00 5.0 91 400 400 400 400 400 Masslynx - Sample List Sample Ust: C:\MASSLYNX\soup-rats.pro\SampleDB\101599a.SPL Printed: Fri Oct 15 11:56:25 1999 _____ Page Position: (1,1) File Name File Text MS File 10MIN-PFOS-POAA' PFOSA-IS 1 101599001 MeOH Blank 10MIN PFOS-POAA--PFOSA-IS 2 101599002 MeOH Blank 10MIN PFOS-POAA'-PFOSA-IS 3 101599003 MeOH Blank 10MIN-PFOS-POAA--PFOSA-IS 4 5 101599004 TOX145, RBL10139-H2O Blank-11, SEE 101599005 TOX145, RBL10139-Uver Blank-11. SEE 10MIN-PFOS-POAA-PFOSA-IS 10MIN--PFOS-POAA--PFOSA-IS 6 7 101599006 TOX145, RBL10139-5ppb-11, SEE 101599007 TOX145, RBL10139-10ppb-11. SEE 10 MIN--PFOS-POAA--PFOSA-IS 10 MIN--PFOS-POAA--PFOSA-IS 101599008 TOX145, RBL10139-25ppb-11, SEE 8 9 101599009 TOX145, RBL10139-50ppb-1 SEE 10MIN-PFOS-POAA--PFOSA-IS 10MIN PFOS-POAA--PFOSA-IS 101599010 TOX145, RBL10139-100ppb-11, SEE 10 10MIN-PFOS-POAA--PFOSA-IS 101599011 TOX145, RBL10139-250ppb-11, SEE 11 10MIN--PFOS-POAA--PFOSA-IS 101599012 TOX145, RBL10139-500ppb-11, SEE 12 10M1N--PFOS-POAA--PFOSA-IS 13 101599013 TOX145, RBL10139-750ppb-11, SEE 10MIN'-PFOS-POAA--PFOSA-IS 14 101599014 TOX145, RBL10139-1000ppb-11, SEE 10MIN PFOS-POAA-PFOSA-IS S ? t5 S15 16 17 18 19 20 21 101999016 101599018 101599019 101599020 101599021 T O X U 5 I RTL-9R03230M, D y l. Control- SEE 10/13/99 RTL-9R03231m ! D y l. Control- SEE 1 0 /13 *9 TOX146. RTL-9R03232M, D y l. Control- SEE W 3 * 9 TOX145, RTL-9R03233M, D yl, Contro- SEE I M 3 * 9 TOX145, RTL-9R03234M, D yl, Control- SEE 1 0 /13 *9 TOX145, RBL10139-250ppb-CCV-11-1, SEE 10MIN-PFOS-POAA--PFOSA-IS 10MIN--PFOS-POAA-PFOSA-IS 10 MIN--PFOS-POAA -PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN -PFOS-POAA--PFOSA-IS 10MIN--PFOS-POAA--PFOSA-IS 10MIN--PFOS-POAAPFOSA-IS 22 23 24 25 26 27 28 IS S l 101599024 101599025 101599026 101599027 101599028 T O X U R i L-9R03235M. Dy4, Control- SEE 1 0 /13 *9 TOX145, RTL-9R03236M, Dy4. Con rol- SEE IW 3 * 9 TOX145, RTL-9R03237M, Dy4, Con ro- SEE IW 3 * 9 TOX145, RTL-9R03238M, Dy4, Contro - SEE 10/13/99 TOX145, RTL-9R03239M, Dy4 , Control- SEE 1W 13*9 TOX145, RBL10139-250ppb-CCV-11-2, SEE 10MIN--PFOS-POAA--PFOSA-IS 10MIN--PFOS-POAA-PFOSA-IS 10MIN -PFOS-POAA--PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN--PFOS-POAA--PFOSA-IS 10MIN--PFOS-POAA-PFOSA-IS 29 30 31 32 33 34 35 101599029 101599030 101599031 101599032 101599033 101599034 101599035 MeOH Blank , ,,-a k ne n TOX145, 9R03230M, D y l, Con ro -250pb-MS-11 TOX145, 9R03230M, D yl, Con ro-250pb-MSD-11 TOX145, 9R03235M, Dy4, Con rol-250pb-MS-12 TOX145, 9R03235M, Dy4, Control-250pb-MSD-12 TOX145, RTL-9R03245M, Dyl ,5mgAig- SEE 10/13/99 TOX145, RBL10139-250ppb-CCV-11-3, SEE 10MIN-PFOS-POAA--PFOSA-IS 10MIN PFOS-POAA--PFOSA-IS 10MIN PFOS-POAA'PFOSA-IS 10MIN--PFOS-POAA--PFOSA-IS 10MIN--PFOS-POAA--PFOSA-IS 10MIN--PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA--PFOSA-IS 36 101599036 MeOH Blank ^ ccp 37 101599037 TOX145, RBL10139-250ppb-CCV-11-3, SEE 10MIN PFOS-POAA--PFOSA-IS 10MIN-PFOS-POAA- PFOSA-IS 38 39 40 41 42 43 44 101599038 101599039 101599040 101599041 101599042 101599043 101599044 MeOH Blank eccm /i-voo TOX145, RTL-9R03246M, D yl. fmgfcg- SEE 0/ 3 * 9 TOX145, RTL-9R03247M, D yl, 5mgfcg- SEE 1W1W99 TOX145, RTL-9R03248M, Dvrt, 5m g*g- SEE W 3 * 9 TOX145, RTL-9R03249M, D y l, 5mgfcg- SEE 1 0 /13 *9 TOX145, RTL-9R03250M, Dy4. 5m g *g -S E E 1W 13*9 TOX145, RBL10139-250ppb-CCV-11-4, SEE 10MIN--PFOS-POAA- PFOSA-IS 10MIN--PFOS-POAA--PFOSA-IS 10MIN-PFOS-POAA--PFOSA-IS 10MIN PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA--PFOSA-IS 10MIN--PFOS-POAA--PFOSA-IS 10MIN--PFOS-POAA-PFOSA-IS 45 46 101599045 MeOH Blank 101599046 TOX145, RBL10139-250ppb-CCV-11-4, SEE 10MIN--PFOS-POAA-PFOSA-IS 10MIN--PFOS-POAA--PFOSA-IS 47 48 49 50 51 52 101599047 101599048 101599049 101599050 101599051 101599052 MeOH Blank TOX145. RTL-9R03251M. Dy4, 5mg4tg- SEE W 3 * 9 TOX145. RTL-9R03252M, Dy4, 5mg/kg- SEE W 3 * 9 TOX145, RTL-9R03253M, Dy4, 5m g*g- SEE 1W1W99 TOX145. RTL-9R03254M. Dy4, 5mg/kg- SEE 1W13/99 TOX145, RBL10139-250ppb-CCV-11-4, SEE 10MIN--PFOS-POAA--PFOSA-IS 10MIN -PFOS-POAA-PFOSA-IS 10MIN--PFOS-POAA-PFOSA-IS 10MIN--PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA--PFOSA-IS 10MIN--PFOS-POAA--PFOSA-IS 53 101599053 MeOH Blank 54 101599054 TOX145, RBL10139-250ppb-CCV-11-4. SEE 10MIN-PFOS-POAA- PFOSA-IS 10MIN--PFOS-POAA--PFOSA-IS 55 101599055 MeOH Blank 56 101599056 TOX145, RBL10139-5ppb-11, SEE 57 101599057 TOX145, RBL10139-10ppb-11. SEE 58 101599058 TOX145, RBL10139-25ppb-11, SEE 59 101599059 TOX145, RBL10139-50ppb-11, SEE 10MIN--PFOS-POAA-PFOSA-IS 10MIN--PFOS-POAA-PFOSA-IS 10MIN PFOS-POAA--PFOSA-IS 10MIN-PFOS-POAA--PFOSA-IS Masslynx - Sample List ` Sample Ust: C:\MASSLYNX\soup-rals.pro\SampleDB\101599a.SPL Printed: Fri Oct 15 11:56:25 1999 Inlet File Bottle Inject Volume Sample Type Cone A 1 10min-10-95 91 2 10min-10-95 91 3 10min-10-95 91 4 10min-10-95 1 5 10min-10-95 2 6 10min-10-95 3 7 10min-10-95 4 8 10min-10-95 5 9 10min-10-95 6 10 10min-10-95 7 11 10min-10-95 8 12 10min-10-95 9 13 10min-10-95 10 14 10min-10-95 11 15 10min-10-95 92 16 10min-10-95 12 17 10min-10-95 13 18 10min-10-95 14 19 10min-10-95 15 20 10min-10-95 16 21 10min-10-95 36 22 10min-10-95 92 23 10min-10-95 17 24 10min-10-95 18 25 10min-10-95 19 26 10min-10-95 20 27 10min-10-95 21 28 10min-10-95 37 29 10min-10-95 93 30 10min-10-95 22 31 10min-10-95 23 32 10min-10-95 24 33 10min-10-95 25 34 10min-10-95 26 35 10min-10-95 38 36 10min-10-95 93 37 10min-10-95 38 38 10min-10-95 93 39 10min-10-95 27 40 10min-10-95 28 41 10min-10-95 29 42 10min-10-95 30 43 10min-10-95 31 44 10min-10-95 39 45 10min-10-95 94 46 10min-10-95 39 47 10min-10-95 94 48 10min-10-95 32 49 10min-10-95 33 50 10min-10-95 34 51 10min-10-95 35 52 10min-10-95 39 53 10min-10-95 95 54 10min-10-95 39 55 10min-10-95 95 56 10min-10-95 3 57 10min-10-95 4 58 10min-10-95 5 59 10min-10-95 6 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- . 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- 10.000 -- -- -- " *** -- " "" Page 2 Page Position: (2,1) Masslynx - Sample List Sample List: C:\MASSLYNX\soup-rats.pro\SampleDB\101599a.SPL Printed: Fri Oct 15 11:56:26 1999 Page 3 Page Position: (1,2) File Name File Text 60 101599060 TOX145, RBL10139-100ppb-11, SEE 61 62 63 101599061 TOX145, RBL10139-250ppb-11, SEE 101599062 TOX145, RBL10139-500ppb-11, SEE 101599063 TOX145, RBL10139-750ppb-11, SEE 64 101599064 TOX145, RBL10139-1000ppl>-11. SEE MS File 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS / Masslynx - Sample List , Sample List: C:\MASSLYNX\soup-rats.pro\SampleDB\101599a.SPL Printed: Fri Oct 15 11:56:26 1999 Inlet File Bottle Inject Volume Sample Type Cone A 60 10min-10-95 7 61 10min-10-95 8 62 10min-10-95 9 63 10min-10-95 10 64 10min-10-95 11 10.000 10.000 10.000 10.000 10.000 -- -- -- -- -- Page 4 Page Position: (2, 2) FACT: DATA REVIEW SUMMARY FORM (V Dale: Data Analyst: Data Review Sign-OfT Analyst Review Name / Date: FACT Study #: Matrix/Timepoints: (/ ^ / / V l T Name/Date: / f l f J J ^ A /o J ^ j ,ifK Simple List: Set-up Analysis Date/Analyst Instrument: A r/? -& 9 A n alyte:. Acceptable Linear Range: e=V*/--$ ) ______ LOQ: c & . ? Q Extraction Blank < k u a . Quality Aaaurance Review Name / Date:_____________ Data Entry:. LAc lohilqq Ci,oomnumnecnntas //Jujusstiufuiccaatuiooinus;: _ _ _ --. (] ) h jM ^ -^ o o p o in tf ^Jrs m o f t - fib 0 ////A a jfa J r ) /?/7Z/7z2_ R"2: A O i W Matrix Blank: C l2 ,U )& . Calibration Checks: 0 6 ^ MS/MSD:_________ Ok Data Status!/ 7 ) txA triA U c ip/ajQ^ d X M L UAa f J o f y>J T f/tr At ,/j/n Wur A P O M U A 'S a Ib T C o f S S - ' h f t F ~7o A ? J f & i r M O - l -7Z&-r AsOL*-rF,____ /V r f /$&>/$$ Analyte: Acceptable Linear Range: 'V . A - ^ 3 _________ A js r r JZj t Xas/h- s>-^y~A4 ,____ LOQ: R"2: f l , Extracted Blank <T ^ Ijb Q j Matrix Blank * -< /* ( & Olts w>X- S^Au-o-rrtr^ t/s U . r*AH- tS-rz~ion~h Calibration Checks: / } / \ f MS/MSD: Data StatusM . J2L fcnWcd [AC loli-xl^ _2 ( J lAnalyte:. l> r > M - Acceptable Linear Range: LOQ:. Extracted B la n k . RA2: Matrix Blank Calibration Checks: M S/MSD:_______ Data Satus: /Tf-V rr M zn J jh ^ c n r ) W- FACT: DATA REVIEW SUMiMARY FORM Dale: Data Analyst FACT Study #: Sample List Set-up Analysis Date/Analyst: Instrument /H lQ ff L . U i ----------------------- Data Review Sign-OfT S g T " ns* u f t I , n uc W shi Quality A m irane Review Name / Date:_____________ Data Entry:. U c id laxh*? Analyte: ^SjY Acceptable Linear Ranse: LOO: --------- - RA2: Calibration Checks: MS/MSD: Data Status: f ib - - . Extraction Blank: ---------- Matrix Blank: ---------- - _______ _ " ----------^ / y ^ o 9 > 9 Q uantify Ccapound l u n u y M p o rt T o i 1 1 9 : b ! m i D i l u t i o n . , M y 1 .1 u.t! /- " '> y -, f0 ^ ) L i " ' 1*"1T tik S ^ L iU I^ 'iiMtothDbMoi* Last aodlfiad: Wd Oot 30 08:16:18 1*89 Job Cedo: Frintod: od Oot 30 00:00:41 1999 1 101999001 2 101999002 3 101999003 4 101999004 5 101999005 6 101999006 7 101999007 6 101999008 9 101999009 10 101999010 11 101999011 12 101999012 13 101999013 14 101999014 15 101999015 16 101999016 n 101999017 18 101999018 19 101999019 20 101999020 21 101999021 22 101999022 23 101999023 24 101999024 25 101999025 26 101999026 27 101999027 28 101999028 29 101999029 30 101999030 31 101999031 32 101999032 33 101999033 34 101999034 35 101999035 36 101999036 37 101999037 38 1 01999038 39 101999039 apiallst fast MaOH T oi" 145: B U 0139-H 20 b lk -1 1 . I x t Skk 10-13-99 T o i 145: R a L 1 0 1 3 9 -L iv .r b lk - 1 1 . t i t SEE 1 0 -1 3 -9 9 T o i 145: 9 B U 0 1 3 9 -S p p b -1 1 , E l t SEE l " " 13: " To* 1 4 5 : R B L 10139-10 p p b - 1 1 , E x t SEC 1 0 - 1 3 - 9 9 To* 145: R B U 0139-2S p p b -1 1 , E x t SEE l " ^ - 9 9 To* 145: RBL10139-50 p pb-11* E x t SEE 1 0 -1 3 -9 9 Tox 145: RBL10139-100 p p b -1 1 , E x t SEE 1 0 *13" " Tox 145: E B U 0139-250 p p b -1 1 , E x t SEE 1 0 -1 3 -9 9 Tox 145: RBL10139-500 p p b -1 1 , E x t SEE 1 0 -1 3 -9 9 Tox 145: RBL10139-7S0 p p b -1 1 , E x t SEE 1 0 -1 3 -9 9 To* 145: RBL10139-1000 p p b -1 1 , E a t SEE 1 0 -1 3 -9 9 MaOH Tox 145: Tox 145: TO* 14 5 : Tox 145: Tox 145: Tox 145: 9R03237M. Day 4 , C o n tr o l, D: 100 9R0324SM . Day 1 5 m q / k q , 0:100 9R03246M. Day 1 , 5 m q /k q , D: 100 9R03247M, 9R03248M, Day 1, Day 1, S m q/kq, 5 m q/kq, D: 100 D:100 RBL10139-250 p p b -1 1 -2 , E xt SEE 1 0 -1 3 -9 9 HaOH Tox 145: Tox 145: Tox 145: Tox 145: Tox 145: Tox 145: 9R03249M. Day 1 , S m q /k q , D :100 9R03251M, Day 4 , S n d /k q , 0 :1 0 0 9R03252M Day 4* S m q / k q , D :1 0 0 9R03253M, Day 4 , 5 m q /k q , D :100 9R032S4M, b a y 4 . S m q /k q , D :100 RBL10139-250 p p b -1 1 -1 , E x t SEE 1 0 -1 3 -9 9 Tox**i45: RBL10139-H 20 b l k - 1 1 , E x t SEX 1 0 - 1 3 - 9 9 Tox 1 4 5 : R M .1 0 1 3 9 -X .iv ar b l k - 1 1 , E x t SBC 1 0 - 1 3 - 9 9 Tox 145: R BL10139-5 p p b -1 1 , E x t SEE 1 0 -1 3 -9 9 Tox 145: RBL10139-10 p p b -1 1 , E x t SEE 1 0 -1 3 -9 9 Tox 145: R M .10139-25 p p b - U , E x t SEE 1 0 -1 3 -9 9 Tox 145: RBL10139-50 p p b -1 1 , E x t SEE 1 0 -1 3 -9 9 Tox 145: RBL10139-100 p p b -1 1 , E x t SEE 1 0 -1 3 -9 9 Tox 145: RBL10139-250 p p b -1 1 , E x t SEE 1 0 -1 3 -9 9 Tox 145: RBL1Q139-S00 p p b - U , E x t SEE 1 0 -1 3 -9 9 Tox 145: RBL10139-750 p p b - U . E x t SEE 1 0 -1 3 -9 9 Tox 145: RBL10139-1000 p p b - U , E xt SEE 1 0 -1 3 -9 9 S tandard S tandard S tandard S tandard S tandard S tandard S tandard S tandard S tan d ard 0C QC S tan d ard S tandard S tandard S tan d ard S tandard S tandard S tandard S tandard S tandard 4 .9 3 9 .7 6 2 4 .8 0 4 9 .3 0 9 7 .6 0 2 4 8 .0 0 4 9 3 .0 0 7 3 5 .0 0 9 7 6 .0 0 4 .9 3 9 .7 6 2 4 .8 0 4 9 .3 0 9 7 .6 0 2 4 8 .0 0 4 9 3 .0 0 7 3 5 .0 0 9 7 6 .0 0 rr 7.159 7 .1 7 1 7 .1 6 7 7 .1 4 0 7 .1 2 3 7.120 7.120 7.137 7.120 7 .1 4 1 7.118 7.120 7.119 7.149 7.119 7.138 7 .1 4 1 7.139 7.139 7.144 7 .1 6 3 7.146 7.145 7.143 7.145 7.168 7.166 7.163 7.191 7.189 7.165 7.140 7.149 7.148 7.120 7.145 7 .1 4 2 7.123 7 .1 4 1 w mu U c . W n JLAcU UiiVk n,ml f 1h'iS n i n w A n u r n W i r i ^ r M 1 ATM 33 29 109 127 266 326 563 778 1265 2818 4996 6355 033 41 3396 2339 3037 3370 2132 2043 25 2630 3050 3897 3395 3570 1805 35 98 118 270 289 498 707 1087 2653 4435 6109 7943 Cone. r i ay a 0. 00 bb 0 . 00 bb 0. 00 bb 0. 00 bb 0 . 00 MX 0. 00 bbx 2 5 . 44 MH S I . 46 MH 1 1 0 . 57 MM 2 9 8 . 68 m 5 6 2 . 73 MM 7 2 7 . 43 MH 930. 73 m 0. 00 bb 368. 79 bd* 240..65 bb 3 2 5 ..31 MM 3 6 5 ..5 9 M 2 1 5 ..5 8 >M 204..85 IM 0..00 b b 2 7 6 ..0 1 IM 3 2 6 .9 1 MH 429..51 bb 368 .6 4 IM 389 .84 bb 176 .0 2 MM 0 .00 bb 0 .00 bb 0 .0 0 M 0 .0 0 bbX 0 .0 0 >MX 17 .5 3 b b 42 .9 2 bb 88 .9 8 MM 278 .8 0 MH 494 .7 5 MM 697 .6 0 MM 919 .7 8 HM %Dv -1 0 0 -1 0 0 3 4 13 20 14 -1 -5 -17 -29 -100 -100 -29 -13 -9 12 0 -5 -6 &vr, W i Uc ic h ilr i .d 3 5 0 fr , O au 5 */Kf r lA C AMlia 062498: Quantitated and Prints by ah 10/20/99 0 s !e E g 1 JKD I s *sw n -4 e f f , 6 , se P =. g, sssasssssS ssssSs ssssss sssSsssssSS 3 P r3T IliliISSI!!Ill l cS l i a i IH s !ITM ^UtV>U>0>n j r - r HE'SE ;;:',,5 t ll l l ll .IH HM 5ESmSSS! ! ! :',,S T s8S85':8 U c m >5555 sS58S:;8 =55?I!? !H S H a i s : 55=5!!!;;? m m m j m rn m JT r" ?- si sigm; Ei 3SSSSS.. ggggggggfc SaaSsss-. ggggggggs -- SI5Ssl255="5S=SSSS=s==ri=SSII5l"-.Is5=3=3 -O O sS ^sasss=S !J!8iissassa L-o O " HgSsSS^-oSSS3oS5ag5SofiSStS--oooog O 5 si;si;i:i:sissrs!isi:ksiii;g5si:iibsssbbss!:bggf |m &&S&S?S&g5m ggX?S?m &3 o cS ~c- J M I I I I HI- ? lr\ o l_ rn T 5 V >o ^ ! ec i I K3 i i I j -fotf ' f u m | m ' o f i q S S tiS K S S S S gS S S X K gS B S S gS tlS C S E C S S .-.*..,,. .* .-. 222222222222222222222223222222222222222^ s s s s s k s s s s ! ss5s s s s s s s s s s s 2Ss s s J S S S S 5 5 5 5 5 5 S s S S S SsHiSS SSSHH SSSSSS ii!! ii iii i m m m i m m m w i mu? m m m p i Sg s - p = j j j j j | 5 { ! > : ; ! ???!!!l;f ?m?i!!bi P - r r r - ts s--'*'-' E" ""' "-? ^ - " . - r r - tc \ ss m p is s "StStSSHHIS`|? I;h I IH55! S5S5S55K*fS? jfff. Jj - T f ^ j v u v ggggggggg g g ggggggggg g iiiiiillil iii i 5 SKSSSSgSSS ggggg gsssgg S S 2 S g g 2 ; g" C \T ~ s: O r or r r or o .r - ssscrssssg g ggggggggggg r .ooooo S S 3 ggggg . o ? o o -O O -- OOO. K gSSSSSSSSS gggggg gggggsgggg K.crs.S t i i i i i tHii I r --Ts Quantify Ceepeund P * e * Y Report Tox 145: Rat aaa, Dllu**d *>y 1*4 a ^ l e Lit: ~ 'C:\*SSfiia\aelia-**ta. f M \ M p l N \ 1 0 1 > Laae aedified: Rad Oct 20 08:31:47 1*#* Method: c:\*U.YMX\aaolia-rata. pRO\MethDB\101999a Laat aedified: Red Oct 20 08:16:18 1099 Job Coda : P rin te d : ed O ct 20 0 9:00:41 1999 Coepound 4: Z8 (Ch2) t Maee 1 101999001 2 101999002 2 101999003 4 101999004 5 101999005 6 101999006 7 101999007 a 101999008 9 101999009 10 101999010 11 101999011 12 101999012 13 101999013 14 101999014 15 101999015 16 101999016 17 101999017 19 101999018 19 101999019 20 101999020 21 101999021 22 101999022 23 101999023 24 101999024 25 101999025 26 101999026 27 101999027 28 101999028 29 101999029 30 101999030 31 101999031 32 101999032 33 101999033 34 101999034 35 101999035 36 101999036 37 101999037 38 101999038 39 101999039 S e r ie lls t te x t MeOH MeOH Tox 1 4 5 : RBL10139-H20 b l k - i : l, E x t SEE 1 0 -1 3 -9 9 Tox 145: R B U 0 1 3 9 -L iw ar b lk -11, E x t SEE 1 0 -1 3 -9 9 Tox 1 4 5 : RBL10139-S ppb-11* E x t SEE 1 0 -1 3 -9 9 Tox 145: RBL10139-10 p p b - ll, , E x t SEE 1 0 -1 3 -9 9 Tox 145: RBX.10139-25 p p b -1 1 ,, E x t SEE 1 0 -1 3 -9 9 Tox 1 4 5 : R B L10139-50 p p b -1 1 ,, E x t SEE 1 0 -1 3 -9 9 Tox 1 4 5 : R B L 10139-100 p p b -1 L, E x t SEE 1 0 - 1 3 - 9 9 Tox 1 4 5 : R B L 10139-250 p p b - l : L, E x t SEE 1 0 - 1 3 - 9 9 Tox 145: RBL10139-S00 p p b -l:l , E x t SEE 1 0 -1 3 -9 9 l , E x t SEE 1 0 -1 3 -9 9 11* E x t SEE 1 0 - 1 3 - 9 9 MeOH Tox 145: Tox 145: Tox 145: Tox 145: Tox 145: Tox 145: 9903237, Dey 4, C o n tro l 0 :1 0 0 9R03245M, Day 1, 5 eg /k g , 9R03246M . Day 1* 5 m q / k q , 9R03247M, Day 1, 5 e g /k g 99032404. Day 1 , 5 m q /kq D: 100 0 :1 0 0 D :1 0 0 D :100 RBL10139-2S0 p p b -1 1 -2 , l * t SEE 1 0 -1 3 -9 9 MeOH Tox 145: Tox 145: Tox 145: Tox 145: Tox 145: Tox 145: 9903249M, Day 1, 5 m q /k q , D:100 9903251M, Day 4, 5 m q /k q , D:100 99032S2M* Day 4 , 5 m q /k q , D :100 9903253M, Day 4, 5 m q /k q , D :100 9903254M* Day 4 , 5 m q /k q , D :100 9B L 10139-250 p p b -1 1 - 1 , E x t SEE 1 0 -1 3 -9 9 Tox 1 4 5 : 9B L10139-K 20 b l k - l l , E x t SEE 1 0 -1 3 -9 9 Tox 1 4 5 : 9 S I .i 0 1 3 9 - l .i w e r b l k - 1 1 . E x t SEE 1 0 - 1 3 - 9 9 Tox 1 4 5 : 9S L 10139-S ppb-11* E x t SEE 1 0 -1 3 -9 9 Tox 1 4 5 : 9BX.10139-10 ppb-11* E x t SEE 1 0 -1 3 -9 9 Tox 145: 9SL 10139-25 p p b -1 1 . E x t SEE 1 0 -1 3 -9 9 Tox 145: 9B L10139-50 ppb-11* E x t SEE 1 0 -1 3 -9 9 Tox 1 4 5 : 9B L 10139-100 pp b -1 1 * E x t SEE 1 0 -1 3 -9 9 Tox 1 4 5 : 9B L 10139-250 p p b -1 1 . E x t SEE 1 0 -1 3 -9 9 Tox 1 4 5 : 9BI.10139-S0O ppb-11* E xt SEE 1 0 -1 3 -9 9 Tox 1 4 5 : 9BL10 1 3 9 -7 5 0 p p b -1 1 * E x t SEE 1 0 - 1 3 - 9 9 Tox 1 4 5 : 9SL10 1 3 9 -1 0 0 0 p p b -1 1 . E x t SEE 1 0 -1 3 -9 9 Type S td Cono S tandard S tandard S tandard S tandard S tandard S tandard S tandard S tandard S tandard 1 .0 0 1 .0 0 1 .0 0 1 .0 0 1 .0 0 1 .0 0 1 .0 0 1 .0 0 1 .0 0 0C QC S tandard S tandard S tandard S tandard S tandard S tandard S tandard S tandard S tandard 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 9T 6.982 6 .9 5 5 6.961 6.958 6.958 6.951 6 .9 6 0 6.956 6.957 6.958 6.934 6.957 6 .9 7 6 6.980 6 .9 7 8 6 .9 5 5 6.984 6.984 6.961 6.912 6 .9 6 0 6 .9 8 3 6 .9 8 0 6.980 7 .0 0 7 7 .0 0 3 6 .9 7 9 6 .9 5 6 6.987 6.963 6 .9 5 9 6.958 6.957 6.961 6 .9 5 5 Ov ( / f ? ) A rea C ene. P lag a IDev 2946 3227 4774 4858 4227 4612 3958 4194 3767 3827 3281 30 36 43 34 32 2585 32 38 28 27 35 2759 8 2979 3288 3941 4388 4134 4085 3571 3937 3460 3218 3342 0.74 bb 0.81 bb 1.20 bb 1.22 bb 1 .0 6 bb 1 .1 6 bb 1.00 bb 1.05 bb 0.95 bb 0 .9 6 bb 0 .8 3 bb 0.01 bb 0.01 bd 0.01 bd 0.01 bd 0.01 bb 0 .6 5 bb 0.01 bb 0.01 bb 0.01 bd 0.01 bd 0.01 bd 0 .6 9 bb 0 .0 0 bb 0 .7 5 bb 0.83 bb 0 .9 9 bb 1 .1 0 bb 1.04 bb 1.03 bd 0.90 bb 0.99 bd 0.87 bb 0.81 bb 0.84 dd -26 -19 20 22 6 16 -0 5 -S -4 -17 -99 -99 -99 -99 -99 -35 -9 9 -9 9 -99 -99 -99 -31 -100 -25 -17 -1 10 4 3 -1 0 -1 -13 -1 9 -1 6 D ala no)' u u l . taf* 4 Aaalla 0C249: Quantitated and Printed by 10/20/99 *' > - *> 9 9 ---------------------- -------------------------------------------------------------------- ^ / y 1 '' *090 1 Quantify Calibration Roport Tox 145: *>4______________________________________ ____________________ _________________________ __________________________ _ iCompouna 1 nameTPFOS Coefficient o f Determination: 0.989844 Calibration curve: 8.25151 * x + 352.987 Response type: External Std, Area ....... Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None 8.41e3n ! Response- /' walla OC24tt: Quanti tatod and trlatod by TM 1 0 / 2 0 / 0 * 0 (^) Quantify Calibration Raport To* 145: Rat: "' Qoy 1_______ ____________________________ ^ _____________ Compoima^ name: PFOSA ~ '' Coefficient o f Determination: 0.997888 Calibration curve: 26.5524 * x + 23.6545 Response type: External Std, Area . Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None 2.60e4-, M I | Response- / / Rap* 2 j/ i I/ IX I 0-k------------------------------ ;--------------------- ;---------- :--- 0.0 200.0 400.0 600.0 Juaalla 0424M: Quantitatod and Rriatod toy 10/20/ (D (^ ) S 800.0 Cone Pi* 3 Ansili 0(2491 : Quiatititad and m a t a d toy * 10/20/99 s t t z . A r & 7 Q u an tify C a lib ra tio n boport T o r 1 4 5 : H o t i - D l l y ^ o n o . Ooy l 4 Compound 4 namiST IS (Ch2) Response Factor: 3976.31 Response type: External Std, Area Curve type: RF 4.86e3-, Wmg* Response- i i / / / 0.80 . 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 Cone 0.9 1.0 Aaoll* 0(3499: Quantitatod and Prlntod by 10/20/9* Method toport Method fila: Last modified: Coapound: Priocd: M :\am aU a-rats.P R O \M ethD e\101999a.m db Ned Oct 20 01:Its19 19990 1 PPOS Thu Oct 21 15:13:12 19 Compound Nus: Internal Ref.: Q uantify Trac: Conc. of Standards: Usar PF Valu: Usr Peak Factor: Integrate Window Factor: Chromatogram nass window: Peak Location totantlon Tis Imins): Relativ Retention Tim: RT Reference: Tina Window (ins): Peak Selection: Baspons Raspons Typ: Response: Calibration Curves Polynomial Typa: Point of Origin: Fit Weighting: Axis Transformation: concentration Units: Moist Pek-to-pak amplitude: Smooth Smoothing: Window sire (scans: Number of smooths: smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: Peak Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: Response Threshold Absolut area: pros (Nona) TIC Cone. A 1.000000p Disabled 1.000000 2 .000 1.0000D 7.17, Enabled 0.000p Disabled (Nona] 0.358 Maarast External Areas Linear Exclude 1/X Nona 100 2 1 30.00 200.00 90.00 Disabled 30.00 1.50. Disabled 0.00. Disabled 2.00. Disabled 0.00. Disabled / h n fix /K -C te & P flZ - to 1 Nethod Report Last modified: Compound: Printed: Wed Oct 20 01:14:16 19990 2: PFOSA Thu Oct 21 15:12:1 1> Compound Name: Internai Rei.: Quantity Trac: Cone, of Standards: Usar RF Vaiu: Uatr Peak Tactor: Integrata Window Tactor: Chromatogram mass window: Peak Location Retencin Time (mina) : Relativo Ratantion Tina: RT Rafranea: Tina Hindow (nina): Peak Selection: Response Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Concentration Units: Noise Peak-to-peak amplitude: Smooth Smooching: Window size (scans): Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: Peak Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative area: Absolut# area: PFQ5A (None! TIC Cone. B 1.000000. Disabled 1.000000 2 .000 1 .00000a 7.124. Enabled 0.000, Disabled (None] 0.262 External Areas Linear Exclude 1/X None 94 Enabled 2 1 30.00 200.00 5.00 0.00 Disabled 30.00 . 1.50, Disabled 0.00. Disabled 2.00. Disabled 0.00, Disabled ( n d n . b S M tf' Page 2 Method Report Method fila: U s t modified: Coapound: Printed: N:\ameUa-reta.PRO\MethDi\101999a.mdb Mad Oct 20 01:1:! I999C 3: PQAA Thu Oct 21 15:13:1 1999 Coapound Name: Incarnai Ref.: Quantify Trace: Cone, of Standards: Usar RF Valua: Usar Peak Factor: Incantata Window Factor: Chroaatogran aass window: Peak Location Ratantion Tina lalns): Relative Retention Time: RT Reference: TiBa Window (Bins): peak Selection: Response Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Concentration Units: Hoise Peafc-to-peak amplitude: Smooth Smoothing: Window size (scans): Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise bsseline maximum: Peak Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: Resoonse Threshold Relative height: Absolute height: Absolute area: NM (Nona] TIC Fixed 1.000000, Disabled 1.000000 2 .0 0 0 l.OOOODa (.941, Enabled 0.000, Disabled (Nona] 0.23 External Rraas Linear Exclude 1/X None 94 Enabled 1 30.00 200.00 90.00 Disabled 30.00 1.50, Disabled 0.00. Disabled 2.00, Disabled 0.00, Disabled Page 3 Method Report Method file: Last Bodlfisd: Compound: rn n u d : K.d Oct 20 0 1 :1 6 : 1 1 1>SC tS (Ch2) Thu Oct 21 15:13:10 19 Compound Name: Internal Ref.: Quantify Trace: Cone, of Standards: User RF Value: User Peak Factor: Integrate Window Factor: Chromatogram mass window: Peak Location Retention Time (mins): Relative Retention Time: RT Reference: Time Window (mins): Peak Selection: Response Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Concentration Units: Noise Peak-to-peak amplitude: Smooth Smoothing: window sire (scans): Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: Peak Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative area: Absolute area: IS (Ch2) INone) TIC Fixed 1.000000, Disabled 1.000000 2 .0 0 0 l.OOOODa .910, Enabled 0.000, Disabled (None] 0.406 Neerest External Areas Linear Exclude 1/X None 94 Enabled 2 1 30.00 2 0 0 .0 0 5.00 90.00 Disabled 30.00 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled >` /fytto&4 Page 4 AMELIA 062498: FACT Equipment Log ,99114 Quattro n, #6448E PAGE DATE: 10/19/99 ANALYST: mmh STUDY NUMBER:TOX145 MATRIX: rat Ever DESCRIPTION:^ FACT Method: ETS-8-7.0 Injection volum e: 10 uL Cycle time: 10 min. Electrode: Z-Spra^ MobUe Phase: 1A12.0 mM NH4CH3CQ2 TN-A- or stndrd number (A) 99085-10-14______ Prepared (date/by): (A) 10/16/99 sah______ Expires: (A) 04/00 ---------------- (B)M eO H __ (B TN-A-2997 (B )10/16/99 sah (B) 04/00 Store at room temp? 0 or N Other:-- Guard column: None ______ _________ Part number: na_________ Lot number._na Analytical column: Keystone B e t a s i l ____ _________________ _______ Size: 2 x 5 0 mm__________ ____ Type:C18__________ Sphere size:J_um--------- Part number: 055-701-2_________ Lot number: P9E11 Serial numben0591816Z Analytical parameters: Drying gas (L/hr): 300 ESI nebulizing gas (L/hr) 10 LC Flow rate: 300 uL/min. Back pressure: 62 bar Sheath gas (L/hr)_0 HPLC solvent gradient: 10min-10-95 Time (min.) 1 ) 0 . 0 0 ____________ 2 ) 1 . 0 0 _______________ 3) 5.50________ 4) 7.50________ 5) 8.00________ %B 100 100 95 0 95.0 10 0 Tuning Method Report Method: C :\MASSLYNX\AMELIA-RATS.PRO\ACQUDB\PFOS1-6KV Printed: Pus Get 19 10:25:49 1999 Page 1 MS SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. Set Rdbk 1.60 40 5 0.2 150 250 1.59 -40 -5 153 248 Pressures Analyser Vacuum Gas Cell Rdbk 1.2e-4 4.6e-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set 15.0 15.0 2.0 0.0 4 650 Set Rd) 14.0 14.0 10 2.0 0.0 40 0 650 11 39 12 canning M t h e d K a p e r t M athod: C : \M M * L Y I(X \A * I^ A -* H . PBO \A CQ tB\ 1CKXM-PO0- nu-za-troiA Lnac Modified: Mon Oct 11 00:22:17 1099 printed: Tue Oct 19 10:22:4 1999 Solvent Dalny ( inn > : 0.00 Function : 1 M M of 1 Mesa f a i r ( U P * ) inter Channel Delay ( Sees ) : Span t Dalton > : Start Tine ( Min ) : End Tine ( Mina ) : Repeat : Channel Parent Daughter 0.03 0.00 0.00 10.00 Dwell (Secs) Coll Energy (eV) 1 413.00 1S9.00 0.30 30 Cone ( V 15 Function : 2 M9I of 1 Me P e a r ( ESP- ) Inter Channel Delay < Secs ) : Span ( Daltons ) : Start Tie ( Mins ) : End Time ( Mina } : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 Dwell (Sees) Coll Energy (V) 1 499.00 99.00 0.30 45 Cone i1 V 0 function : 3 M M of 1 Mesa F a i r ( B SP - ) Inter Channel Delay ( Secs ) : Span ( Daltons ) : Start Tine 1 Mins 1 : End Tlee ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 Dwell (Secs) Coll Energy laV) 1 427.00 10.00 0.30 40 Cone < V 0 Function : 4 M M of 1 M s s P a ir ( U P - ) Inter Channel Delay 1 Secs ) : Span ( Daltons ) : Start Tiae ( Mins ) End Tine { Mins } : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 Dwell (Seca) coll Energy (aV) 1 499.00 79.00 0.40 Cone ( v 0 Masslynx - Sample List Sample List: C:\MASSLYNX\amelia-rats.PRO\SampleDB\101999a-SPL Printed: Tue Oct 19 14:10:27 1999 /O /'? ? / Page 1 Page Position: (1,1 ) File Name File Text MS File 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 101999001 101999002 101999003 101999004 101999005 101999006 101999007 101999008 101999009 101999010 101999011 101999012 101999013 101999014 101999015 101999016 101999017 101999018 101999019 101999020 101999021 101999022 101999023 101999024 101999025 101999026 101999027 101999028 101999029 101999030 101999031 101999032 101999033 101999034 101999035 101999036 101999037 101999038 101999039 MeOH MeOH Tox 145: RBL10139-H2O blk-11, Ext SEE 10-13-99 Tox 145: RBL10139-Liver blk-11. Ext SEE 10-13-99 Tox 145: RBL10139-5 ppb-11. Ext SEE 10-13-99 Tox 145: RBL10139-10 ppb-11. Ext SEE 10-13-99 Tox 145: RBL10139-25 ppb-11, Ext SEE 10-13-99 Tox 145: RBL10139-50 ppb-11, Ext SEE 10-13-99 Tox 145: RBL10139-100 ppb-11, Ext SEE 10-13-99 Tox 145: RBL10139-250 ppb-11. Ext SEE 10-13-99 Tox 145: RBL10139-500 ppb-11. Ext SEE 10-13-99 Tox 145: RBL10139-750 ppb-11. Ext SEE 10-13-99 Tox 145: RBL10139-1000 ppb-11. Ext SEE 10-13-99 MeOH Tox 145:9R03237M, Day 4, Control. D:100 Tox 145: 9R03245M, Day 1. 5 mg/kg, D:100 Tox 145: 9R03246M. Day 1 .5 mg/kg. D:100 Tox 145:9R03247M. Day 1 .5 mg/kg, D:100 Tox 145:9R03248M. Day 1 ,5 mg/kg. D:100 Tox 145: RBL10139-250 ppb-11-2. Ext SEE 10-13-99 MeOH Tox 145: 9R03249M, Day 1 ,5 mg/kg. D:100 Tox 145:9R03251M. Day 4 .5 mg/kg, D:100 Tox 145: 9R03252M, Day 4, 5 mg/kg, D:100 Tox 145: 9R03253M, Day 4, 5 mg/kg, D:100 Tox 145: 9R03254M, Day 4, 5 mg/kg, D:100 Tox 145: RBL10139-250 ppb-11-1, Ext SEE 10-13-99 Tox 145: RBL10139-H2O blk-11. Ext SEE 10-13-99 Tox 145: RBL10139-Uver blk-11, Ext SEE 10-13-99 Tox 145: RBL10139-5 ppb-11. Ext SEE 10-13-99 Tox 145: RBL10139-10 ppb-11, Ext SEE 10-13-99 Tox 145: RBL10139-25 ppb-11. Ext SEE 10-1399 Tox 145: RBL10139-50 ppb-11. Ext SEE 10-1399 Tox 145: RBL10139-100 ppb-11. Ext SEE 10-13-99 Tox 145: RBL10139-250 ppb-11. Ext SEE 1313-99 Tox 145: RBL10133500 ppb-11, Ext SEE 1313-99 Tox 145: RBL10 1 3 37 5 0 ppb-11. Ext SEE 1 3 1 3 9 9 Tox 145: RBL101331000 ppb-11. Ext SEE 1 3 1 3 9 9 10MIN-PFOS-POAA-IS-PFOSA 1 0 MIN-PFOS-POAA-IS-PFOSA 1 0 MIN-PFOS-POAA-IS-PFOSA 1 0 MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 1 0 MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 1 0 MIN-PFOS-POAA-IS-PFOSA 1OMIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 1 0 MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 1OMIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 1 0 MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA Masslynx - Sample List Sample List: C:\MASSLYNX\amella-rats.PROVSampleDB\101999a.SPL Printed: Tue Oct 19 14:10:27 1999 Page 2 Page Position: (2 ,1 ) Inlet File Bottle Inject Volume Sample Type Cone A Cone B C o ncC C oncD Cone E Cone F 1 10min-10-95 91 2 10mirv10-95 91 3 10min-10-95 1 4 10min-10-95 2 S 10mirv10-95 3 6 10min-10-95 4 7 10min-10-95 5 8 10min-10-95 6 9 10mln-10-95 7 10 10min-10-95 8 11 10min-1O-95 9 12 10min-10-95 10 13 10mirv-10-95 11 14 10min-10-95 91 15 10min-10-95 12 16 10min-10-95 13 17 10mirv10-95 14 18 10min-10-95 15 19 10mir>-10-95 16 20 10mirv10-95 81 21 10mirv10-95 92 22 10mln-10-95 17 23 10min-10-95 18 24 10min-1O-95 19 25 10min-10-95 20 26 10min-10-95 21 27 10min-10-95 82 28 10min-10-95 92 29 10min-10-95 1 30 10min-10-95 2 31 10mln-10-95 3 32 10min-10-95 4 33 10mir>-10-95 5 34 10min-10-95 6 35 10min-10-95 7 36 10min-10-95 8 37 10min-10-95 9 38 10min-10-95 10 39 10min-10-95 11 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- FACT: D A T A REVIEW SUMMARY FORM fo (jL- ' A D ate : D ata Analyst: T Data Review Sign-Off ' A nalyst Review Name /D ate: . IfT i f a F A C T S tu d y : // S ' - m J v M atrix/Tim epoints: 7 * Jveir C u rte- -- cM-. //zih1 & ) Sample List: /O Z f f C S et-up Analysis D ate/A nalyst Instrum ent / h /? 9 7 A '. 0 2 / fa' Analyte: _ Tq a a C a t t yG> A c c e p ta b le L in e a r R a n g e : ___ LOQ: U ___ R -2: 0.1U f M ______ C alibration C hecks: X /n M S / M S D :_____ D ata Status: JA. aj/a E xtractio n B lanlc^ / d a / r 'U**-LSQ M a tr ix B la n k : /jre*f `4i+*-C T echnical Review N am e / D ate: /atn/Ql Q uality A ssurance Review N a m e / D a te :_______________ D ata E n try : _ A)e * r U M lolillW C o m m e n ts / J u s t i f i a i t i o n s : i________________ 7ZI ./3-j j L . f2~3o^,L , *--</ ^>-7 T9ii- LH-rt. Sr-**-- ' M a C*fUr-tMC-r- riLC. o - t i n t s -i/JUC J i* . t'**. r- K< L J 4 h . - la- tx-dc*------ -fi J e t g. y* oJ-l* at- tUame. '-Loa-- 0 - i r - ~fc<- fitM.u pomt~ Mi-S--Otdsdc o-f -fa. Lpn-.s Ir-k^r, t -/a. b a l ' ------- Analyte: TfS, -H7} A c c e p ta b le L in e a r R a n g e : /Z -^OjjL > ------------------- LOQ: 2.3$j >L E x tra c te d B la n k : ess La*. 0(1 R * 2 : Q . f t l t e Z - __________ M atrix Blank: / La* l O Q C a lib ra tio n C h e c k s : H A _________________________________________________ M S/M SD : D ata Status: JjjA. Al Analyte: w A cceptable L inear R ange: M & L O Q : ____ H t _________________ R A2 : UA-_________________ C a lib ra tio n C h e c k s : efa M S / M S D :___ D ata Satus: A3M lo)A E xtracted Blank: tt M atrix Blank: / / A IAC IQItflW fi v u * J ) 4 - - - T a s - * / z < / ? y _____ A r t e ------------- Co m a v X> r {aj^ a t a ./kJ. 't e l i s i # ^ 7 e - L -l'ftjL pat'-J-* s /Irojyxel-------- '/ V a R - -M e. tu.nrc 4,6 4 U I - t u /-X J A . i s t J j tu- less t * * - 4a Q . ~LL*. M t jfij l ./ , / t . f d * J t o n d * ut**. d i L l u . r i r e_/____/_K_.____r_d__c ,- yh . J j y o t c a x___ n [ vahuasQ j s j / i t u & s r a t t < k jt- tL f a v tr e % *a s L U * , 4 L ^ ^ i h ex. r a lo th J fa x c s b ld - l u . fb-C) BIIC ko -J - rieuiasf'''- Q J/a. I l tS ka l ioki 4i* Je\ll4l*- * k - -M ik-d 0fk- k ' ~^*s J FACT: DATA REVIEW SUMMARY FORM l/p . Dale: Data Analyst' FACT Study#: Matrix/Timcpoints: Sample L ist C Set-up Analysis Datc/Analyst Instrument /o /z g /k 3+ s -iculia, O i *1 f t mi - Analvte: T f ^ A Acceptable Linear Range: LOO: R*2: ________ Calibration Checks: //A ______ MS/MSD: MA Data Status: J L v jvJ> Extraction Blank: ! ts 4 L * `*-tO- Matrix Blank: -Uhl*. >3. Data Review Sign-OfT Analyst Review^ r Name / Date: J A S t /u ( W Technical Review Name / Date:____ EJtr 4t> [ fl U tl lo/zii^l Quality Assurance Review Name / Date:____________ Data Entry: Aio _____(AC- i of C om m ents/Justifications:__________________________ _ L M c J h-S>Sbjji P o t w b Jh oojjrj^LL tfJf &>> ''ijh'l &-f4-' 4'lbie l_ _ / b o _ * L p u Jr Liin-ks L/auJj lo Q _ MdL*.ka ! U h* Sa y- fpySA _____ Ik y * J a is L b jL - I k s . t - > / u , / f `} -------------- C ) P*>2 m & - o e * c r r , o r J A / p n * > t t -r*> < s r o c o < ? c d ----- - T T s r r j j / z j i o ^ - r - i , . / T O & r / o l j J . * aaataiaaa I *: rtOnnr hOTkJh'OMtJh^Oi'iOtUJThI'MO sssssssss 5 5 5 5 - 3 ,3 5 `3 UUUliUUUtJli nnMinninn S1 i et * on 28 %\ ` If * srt ^ S^ u g-ij- .3 38SS ISIS S8 MflkN sW ii sV J U h s O M si 3 .. 1 14 w + * 12 4 4 ;! J j iE3 U"Hl"I3 S il^ ^ ! Nn eS K tfinAsifi>ttAN \H^>*ISSSNN 4N N N S 555M?hh-aV.VaaVaVpJi o if& S fS S S328S2SSS5 H NNNNUNNNNNN f NNNNNNNNNN N oooooeooooo sssaaaaaaaaaaa I liliiiiiiiiiii 1 tnsitntnsiifitn'nrtintntn NNNNNNNNNNNNM OOOOOOOOOOOOO 3 s L 1 S n m a 3 e 1 r e t i I Ti 0 i 5 KOIKO>KO)KOiKO>KO)KOIKOtKOiOK>OK)OK)OK>f| ltfVIDKISltlStf itlf OOOOOOOOOOOOO ssessssss!r p p p f p p r t `r*ritr OOOOOOQOOOO NMMMNNMMMMM NNNMNNKINKINM H f R TT i i i <t i t Ne3o3e sw o lofwsv? & i t *--*- (p **** M k* - a)r ' f >-- O3 I HNHOOOVITK MOOOOSWM I OVSSSMtJMNM SMNNMKIMMS' H NNMMKISNN O Ks v s 'm i ( O h s --OM o m -M ,3 3 MUUUUWMWW ftftftftftrfftft/t 5S5555S5* eem&&& aaao.aao.aa NUH O- a. 4 K K O H C Ot-OHHK 3 0*HH J J U I acr ccrr ec XX> Jo o o o o x 6m8 ii; ff* g! N 7 I ! p se i i 9 ? m rn m s*A 5O SS I SSSS s s s s ! 5 gssssiS s s s s s s s s s SSggggSgSSS ? 3 U i m 0 e m ? e s 1 i I 9 i ? SScSSk e . gggggSgSE 3333333333s3ss SsSSsSss3 H Ss s k ; . ^ ss g ssibsississs? ggggggggggggi . i : : . .ss I Quantify Calibration taport T0X14S*rabbit U w r curva- ait. 10/22/ Compound 1 name: POAA (C hi) Coefficient o f Determination: 0.996986 Calibration curve: 0.253166 * x + 36.3287 " f U l" ? f .H [ ** Am Ii 0(249: Quantitated and printed by iaa 10/24/9# Q uantify C a lib ra tio n R aport ___ TGX 14S-rabtoit li v o r o u rv o - u t . 1 0 /2 2 /9 9 W * Compound 2 name: PFOS (Chi) Coefficient o f Determination: 0.992922 Calibration curve: 6.34685 * x + 149.692 9*9* 2 AMlla 0(2499: Quantitated and printed by iaa 10/2C/99 Quantify Calibration M p o r t TOX14S-rabbit livor curvo- out. 10/22/99 Compound 3 name: IS (Ch3) Response Factor 2378.96 :Response type: External Std, Area Curve type: RF 2.73e3-, I Response- Paga 3 I / o l 5 OJ Amlia 0(2499: Qgantltatod and printed by iaa 10/29/99 0 0.5 0.6 0.7 I -- Cone 1.0 Quantify Calibration Report TOX14S-rabbit livor curvo- u t . 10/22/ Compound 4 name: PFOSA (Ch4) Coefficient o f Determination: 0.996087 Calibration curve: 17.5980 * x + 76.6733 Response type: External Std, Area . . . __ Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None Psg* 4 AMlla 0(2491 : Quantitated and printed by laa 10/2(/9 Method Report Httnod ill.: l4 j c a o d i f i e d : Compound: Printed: C :\HXS3LY11X\M. 11*062491 PRO\M .th D B \l0 2 5 9 9 c . d b Tue O ct 26 0 9 :3 4 :4 2 1999C 1: P O M (Chi) Tue Oct 26 09:44:34 1999 Compound Name: Internal Ref.: Quantify Trace: Cone, of Standards: (Jeer RF Value: User Peek Factor: Integrate Window rector: Chromatogram mass window: Peak Location Retention Time (mins): Relative Retention Time: RT Reference: Time Window (mins) : Peak Selection: Response Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: n t weighting: Axis Transformation: Concentration Units: Noise Paak-to-peak amplitude: Smooth Smoothing: Window size (scans): Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: Peak Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative area: Absolute area: POM (Chi) (Nona] TIC Cone. B 1.000000 Disabled 1.000000 2.000 1.00000a 6.1*9, Enabled 0.000, Disabled (None] 0.2S2 Nearest External Areas Linear Exclude 1/X None 91 Enabled 1 30.00 200.00 5.00 90.00 Disabled 30.00 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled Hetnod Report MCH0d fll E LdlU.d: Compound; Printed: C: \MA2SLYNX\Mli,062498.PRO\MthDB\ 102 599c. db TU. Oct 26 06:24:42 1999C 2: PF05 (Ch2) Tue Oct 2 09:44:34 1999 Compound Null: Internal Ref.: Quantify Trace: Cone, of Standard: User AT Valua: User Peak Factor: Integrate window Factor: Chromatograemass window: Peak Location Retention Tine tains): Relative Retention Tiae: RT Reference: Tlae Window (mins): Peak Selection: Resoonse Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Concentration Units: Noise peak-to-peak amplitude: Saooth Smoothing: Window sire (scans): Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline aaximua: Peak Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: Resoonse Threshold Relative height: Absolute height: Relative area: Absolute area: PFOS ICh2) (Hone] TIC Cone. A 1.000000 Disabled 1.000000 2.000 1 .OOOODa 7.109 Enabled 0.000, Disabled (None] 0.227 External Areas Linear /xExclude 1 None 96 Enabled 2 1 30.00 200.00 5.00 90.00 Disabled 30.00 * 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled H.tRod Raporc Method flit: Last nodifltd: Compound: Print.d: C:\MMSI.TOX\Mli*06249l .PRO\M,thDU02599c.dlj Tu. Oct 26 09:34:42 1999C 3: IS (Ch3) Tu. Oct 26 09:64:34 1999 Coapound Haas: Internal Ref.: Quantify Trace: Cone, of Standards: User RF Value: User Peak Factor: Integrate Window Factor: Chromatogram aass window: Peak Location Retention Time (ains): Relative Retention Tine: RT Reference: Tiae Window (ains) : Peak Selection: Response Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: Fit weighting: Axis Transformation: Concentration Units: Noise Pesk-to*peak amplitude: Snooth Saoothing: Window size (scans): Nuabar of snooths: Smoothing aethod: Baselines Join valley threshold: Reduce peak tailing: Raisa baseline aaxiaua: Peak Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative area: Absoluts araa: ZS (Ch3) (Nona] TIC rued 1.000000 Disabled 1.000000 2.000 l.OOOODa 6.924, Enabled 0.000, Disabled (None) 0.252 Nearest External Areas Linear Exclude 1/X None 74 E n a b le d 2 1 30.00 2 0 0 .0 0 5.00 90.00 Disabled 30.00 1.S0, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled Method Report Method file: L*sc modified: Compound: Printed: C:\NASSlYKX\amelia092498.PRO\MethDB\102S99e.mdb Tu* Oct 26 09:34:42 1999C 4: PFOSA (CM) Tue Oct 2 09:44:34 1999 Compound Name: Internal hit.: Quantify Trace: Cone, of Standard*: User RF Valuo: User Peak Factor: Integrate Window Factor: Chromatogram mass window: Peak Location Retention Time (mins): Relative Retention Time: RT Reference: Time Window (mins): Peak Selection: ResDOnse Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Concentration Units: Noise peak-to-peak amplitude: Smooth Smoothing: Window size (scans): Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: Peak Scoaratlon Draw vertical threshold: Detect shoulders: Shoulder threshold: ResDonse Threshold Relative height: Absolut* height: Relative area: Absolute area: PFOSA (CM) (None] TIC Cone. B 1.000000, Disabled 1.000000 2.000 l.OOOODa 7.951, Enabled 0.000, Disabled (None) 0.311 External Areas Linear Exclude 1/X Mon* 319 Enabled 2 l 30.00 200.00 5.00 90.00 Disabled 30.00 ' 1.S0, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled AMELIA 062498: FACT Equipment Log *99114 Quattro U, #6448E PAGE DATE: 10/25/99 ANALYST: ias STUDY NUMBER: TOI45 MATRIX: Rabbit Liver DESCRIPTION: Curve FACT Method: ETS-8-7.0 Injection volume: 10 uL Cycle time: 10 min. Electrode: Z-Spra^ Mobile Phase: (A)2.0 mM NH4CH3CQ2 (B) MeOH TN-A- or stndrd number (A) 99085-11-3______ (B) TN-A-2945 Prepared (date/by): (M 10/21/99 sah______ fB) 10/20/99 ias Expires: (A) 04/00 _____________ (B1 04/00 Store at room temp? [Y] or N Other-- Guard column: None _________________ Part number: na________ Lot numberj a Analytical column: Keystone Betasil ____________________________ Size: 2 x 5 0 mm_______________ Type:C18__________ Sphere size:Jum--------- Part number: 055-701-2_________ Lot number: P9E11 Serial number:0591816Z Analytical parameters: Drying gas (L/hr): 300 ESI nebulizing gas (L/hr) 10 LC Flow rate: 300 uL/min. Back pressure: 62 bar Sheath gas (L/hr)_0 HPLC solvent gradient: 10min-10-95 Time (min.)____ 1 ) 0 , 0 0 ____________ %B 100 2 ) 1.00 ____________ 3) 5.50________ 4) 7.50________ 5) 8.00________ 100 95.0 95.0 iM . Tuning Method Report Method: C : \M ASSLYNX\AM ELIA-RATS.PRO\ACQUDB\PFOS1 - 6KV Printed: Mon O c t 25 1 0 :1 3 :5 8 1999 Page 1 SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Desolvation Temp. Temp. Set Rdbk 1.60 40 5 0.2 150 250 1.60 -60 -6 151 250 Pressures Analyser Vacuum Gas Cell Rdbk 1.2e-4 4.5e-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set Rdbk 15.0 15.0 2.0 0.0 4 650 7 S e t Rdbk 14.0 14.0 10 2.0 0.0 40 0 650 46 39 48 Scanning Method Rapert i H.U.O,,; c: * e \ M W D * \ KKD.-PfO.-tOX*- If-F I M * Laae Modified: Mon Oct 11 0i22:17 1*** Printed: Mon Oct 25 10:13:30 ! Solvent lay ( aUne ) : 0.00 Function : 1 MM o f 1 Maas P a ir C U P - > Inter Channel Delay ( Seca ) : Span ( Daltons ) : Start Tiaa < M m s ) : End Tiae < Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0 .0 0 10.00 Dwell (Seca) Coll energy <aV) 1 413.00 169.00 0.30 30 Cone ( v ) 15 Function : 2 M M of 1 Maaa P a ir ( U P - > Inter Channel Delay I Secs ) : Span ( Daltons ) : Start Tiae < Mins ) : End Tiae Mina ) : 0.03 0.00 -00 10.00 **p Channel Parent Daughter I*ell (Secs) Coll Energy (eV) Cone ( V ) 1 499.00 99.00 0.30 45 < Function : 3 MM o f 1 M ae P a ir ( U P - ) Inter Channel Delay { Secs I : Span < Daltons ) : Start Tiae I Mins ) : End Tiae ( Mins ) : 0.03 0.00 0.00 10.00 B*P**,Chinn.l Parent Dnuqhc.r D m 11 IS.ca) Coll En.rqy I.V) Con. ( V I 1 427.00 60.00 0.30 40 * Function : 4 I of 1 toss Pair ( UP-* ) Inter Channel Delay I Secs ) : Span ( Daltons ) : Start Time ( Mins ) : End Tiae ( Mins ) : Repeats CChannel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) Coll Energy (eV) 1 498.00 70.00 0.40 45 Cone ( V ) 80 Method Report Method File: Last Modified: Printed: c : \m a s s l y n x \ a m e li a - r a t s .p ro \a c q u d b \1 0 m in -1 0 - 95 Monday, October 25, 1999 10:12:15 Monday, October 25, 1999 10:13:44 Page 1 HP1100 LC Pump Initial Conditions Solvents A% B% C% D% Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 90.0 10.0 0.0 0.0 0.300 10.0 0 400 30.0 30.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 5 entries which are Time 0.00 1.00 5.50 7.50 8.00 A% 90.0 90.0 5.0 5.0 90.0 B% 10.0 10.0 95.0 95.0 10.0 C% 0.0 0.0 0.0 0.0 0.0 HP1100 LC Pump External Event Timetable The Timetable contains 3 entries which are : Time Initial 0.00 0.10 Column Switch Contactl Off Off Off On Off Off Contact2 Off On Off D% 0.0 0.0 0.0 0.0 0.0 Contact3 Off Off Off Flow 0.300 0.300 0.300 0.300 0.300 Contact4 Off On Off Pressure 400 400 400 400 400 HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (/il/min) Draw Position (mm) Stop Time (mins) Injection Volume(^1) Vial Number 22 0000.0 0.00 9.00 10.0 13 Masslynx - Sample List Sample Ust: C:\MASSLYNX\amelia-rats.PRO\SampleDB\102599c!SPL Printed: Mon Oct 25 10:13:12 1999 Page 1 Page Position: (1,1) File Name File Text MS File Inlet File 10MIN-PFOS-POAA-IS-PFOSA 10min-10-95 1 102599035 MeOH Blank 10MIN-PFOS-POAA-IS-PFOSA 10min-10-95 2 3 4 5 6 7 8 9 10 11 12 13 102599036 102599037 102599038 102599039 102599040 102599041 102599042 102599043 102599044 102599045 102599046 102599047 MeOH Blank _ TOX145-RBL10229-H2O Blank-1,10/22/99 RWW TOX145-RBL10229-Liver Blank-1,10/22/99 RWW TOX145-RBL10229-5ppb-1,10/22/99 RWW TOX145-RBL10229-12ppb-1,10/22/99 RWW TOX145-RBL10229-30ppb-1,10/22^99 RWW TOX145-RBL10229-60p pb -1,1/2^ 9R W W TOX145-RBL10229-120ppb-1,10/22/99 RWW TOX145-RBL10229-300ppt>-1,10/22/99 RWW TOX145-RBL10229-600ppb-1,10/22/99 RWW TOX145-RBL10229-900ppb-1. 12/W RWW TOX145-RBL10229-1200ppb-1,10/22/99 RWW 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10min-10-95 10min-10-95 10min-10-95 10min-10-95 10min-10-95 10min-10-95 10min-10-95 10min-10-95 10min-10-95 10min-10-95 10min-10-95 Bottle Inject Volume 1 92 2 92 3 12 4 13 56 14 15 7 16 8 17 9 18 10 19 11 20 12 21 13 22 10 10 10 10 10 10 10 10 10 10 10 10 10 Date: Data Analyst FACT: DATA REVIEW SUMMARY FORM Data Review Sign-OfT Analyst Review . Name / Date: S ,9f z l f l 1 p*. U 2 IAC_ u lw in FACT Study H: T*NS. Matrix/Timepoints: 'TLclk. Z d " /fo it Qn d h n + d r o * , Sample Lilt / 0('f9`la Set-up Analysis Date/Analyst Instrument fo /zifa ^ 1 F & z ifl fa ft Analvte: ToA A C & n')P Acceptable Linear Range: LOO: lo r v i R-2: f.DjJ, - Extraction Blank: }JA Matrix Blank: AW Calibration Checks: MS/MSD Data Status: J3 / m k- f J o J ( f t i i ' f t d --- Q & L V - b l t f f a - 11 Quality Assurance Review Name / Date: Data Entry-: K b / W fo s fo r iv i G *L u h f f f Comments / Justifications: ^ vfc- 2 j j .I c J ' T & Z j r L C i Y ^ J b u d s ____ lu t * * fn -J>v^,n<L 6- f '***' ___ iLe. fjL ru* .< h 4 h c e ltv itc f t* A 3 s i L laU -es U t J - A O fv -e - 4a /^S5~ 7L Ko U d ^ -k s -A e d r / z d - Cm / LhJL. 4L tun*. ''b in ___ Analyte: ffi> 6 Acceptable Linear Range: h LOO: .O ly v l R-2: Q .W S iS - CalibrationIChecks: fiUk-~- Extracted Blank: A iA Matrix Blank: ^4 ----------- MS/MSD: Data Status: N tt U p n i t d * tL thl^ 3 ^Analyte: TfcrfA CCHs'') Acceptable Linear Range: y LOQ:. R"2: Extracted Blank: Matrix Blank: / / 4 Calibration Checks: MS/MSD 3 Data Satus: D dk m ^ ~]Ll. S'os j j L *J ^SS^' l , <-io e jr e r [ v o } f> d - tv j j L - J jl fry's m f L e -Prf- Q . J Vh. i .he.j> JC. oof, A' x t i a S JIe hNLi -[->**- / e S S __ -- > 'V o t ~ J b Im o * * ' h J f J L - Cuvue.- 3 L X* MAve U a.h'* i-a 6*4<o-d /L--J k ie K _ ISJf-fLs - fh _ S * 4 -- I x s > 4 ? l/t1 ___________________ Q > 7 L / . v ijp L . S'- 8 jj> L * /! jJ h . to -- *D>b 'P a d s te r * J r o V J < J lo e c a u & e -__ 4 ito ta J J tu ta } -> o * -* 'f r ^ ___ exix. (J -e J (t*C- o f Mioy* 1 "So rMyt^jsltS luCtr -fio a. >*-tS a J c u < w { s L o i-J h u p-d - W ^ e - Z e r / ^ !hS >aJ ^ b er* fu ti- N X k w / -0 fa ? # 6 U t , , rL , m y U fh r l D u i ^ o u r s W z p tx r j c tu u U fa fiJ - f v m ^ w y t b in s a u f & fw ( f a (J & M U l i f t I f f Dale: Data Analyst 0o, f o / tL . 3*s FACT: DATA REVIEW SUMMARY FORM Data Review Sign-OfT Analyst Review Name / Date: lof?- l*C u lo rjil FACT Study*: Matrix/Timepoints: 7ox//:f _ & ~ j *u. cskSt/ko.4i >- Sample List Set-up Analysis Date/Analyst Instrument . fa h i / / * $ Spy * y $ /i9 Analyte: Acceptable Linear Range: LOQ: Ma _________ RA2 :________ //A _________ Calibration Checks: M S /M S D :______ Data Status: ________________________ Extraction Blank: A/A Matrix Blank: H * Technical Review Name / Date: Quality Assurance Review Name / Date: Data Entry: Comments / Justifications: Q ) xs C o h l + A * [b o Ct-J siL&ieJed' A * u y / ~ fL e. L a J a * -c+ . L c L __ k>e**- J u U iX- tLs SjoO 1&* e/ -4 U ______ r e a - C a n * - J % f a - - jL*-_________ d r o p y tj fijU -J-H I ~ fU t e d . / C u - r t K . - /n _____ $ A--//--A- iC rtLS ***-< lr. f J u a . ' S r v t e H i u : 'i'l* &r*JU m J U j_ J u.q h v &`S Ic a a J J J ,/a - r g y c c i L e. / j j j / f faa se-fjcfva.cJ< efa- o - ^ tJ t r u i *., 'faj-g. s L J l JCo-/ ta* rt*Ag/- U S ' "A *}/??_________________________ Quantify Cutiound I t a i i y Kapert pros/nou/iou a*t. /*/* iTGX14S-twaan 10 doit ooafiraatioi 10 I ^ U Lilt : C: \MBS8LT1CC\aoup020199 .pro\lM1 iflBX10ai99a Lait nodifiad: Pri Oct 39 07:03:5 1999 Matted: C:\MKMLnot\aeup030199.preXMethfleM03999a Laat oodlfiad: Fri Oct 39 06:83:35 1999 Job Coda: Printad: Frt Oct 39 07:37:35 1999 Conpound 1: N I A (Cfel) Mm 1 102899001 3 103899002 3 102899003 10289900 5 10289900S 6 102899006 7 102899007 8 102899008 9 102899009 10 102899010 11 102899011 12 102899012 13 102899013 11 10289901 15 102899015 16 102899016 17 102899017 18 102899018 19 102899019 20 102899020 21 102899021 22 102899022 23 102899023 2 10289902 25 102899025 26 102899026 27 102899027 28 102899028 29 102899029 Ba^lalist Taut KeOH Blk MaOB Blk ratiX`99086-63-1, lppb- 9/10/99 BMW FCKijt-99086-43-2, Sppb- 9/10/99 BMW P O U jc-99086-43-3. lOppb- 9/10/99 BMW FCKix-99086-43-4. 2Sppb- 9/10/99 BMW FQtix-99086-43-5, 50ppb- 9/10/99 BMW FGHix-99086-43-6. lOOppb- 9/10/99 BMW FQJC-99086-43-7, 250ppb- 9/10/99 BMW FQlijc-99086-43-8, SOOppb- 9/10/99 BMW PCHiJ(-99086-3-9. 750ppb- 9/10/99 BMW MaOB Blk TOXl*5-PrOS/PCXA in Tween-doe-2ppb- 10/28/99 IAS TOX15-PPOS/PQAA in TVaan-na-ppb- 10/28/99 ZAS POiix-99086-43-4, 2Sppb- 9/10/99 BMW MaOB Blk TOX145-PFOSA in Twen-doae-rlOOppb- 10/28/99 ZAS TOX145-PFOSA in PCKix-99086-43-7 2S0ppb- 9/10/99 BMW MaOB Blk PCKJ(-990B6-43-l FQIix-99086-43-2, FQIix-99066-43-3 PQx-99086-43-4 PGMX-99086-43-S rOtiJC-99086-43-6 PQtLx-99086-3-7 PQlix-99086-43-8 rOti-x-99086-43-9 lppb- 9/10/99 BMW 5ppb- 9/10/99 BMW lOppb- 9/10/99 BMW 25ppb- 9/10/99 BMW 50ppb- 9/10/99 BMW lOOppb- 9/10/99 BMW 2S0ppb- 9/10/99 BMW SOOppb- 9/10/99 BMW 7S0ppb- 9/10/99 BMW Standard Standard Standard Standard Standard Standard Standard Standard Standard QC OC Standard Standard Standard Standard Standard Standard Standard Standard Standard ltd Cene 1.00 5.02 10.00 25.10 50.20 100.00 251.00 502.00 752.00 2S.10 251.00 1.00 5.02 10.00 25.10 50.20 100.00 251.00 502.00 . 752.00 KT 7.043 7.107 7.085 7.087 7.092 7.085 7.110 7.102 7.131 7.106 7.130 7.125 7.129 7.111 7.106 7.132 7.128 7.126 7.130 7.157 7.125 7.130 7.133 7.128 7.129 Araa Plagi cone. %Dmr 17 KM 38 bb 87 MM 193 bb 364 bb 743 bb 1780 bb 3005 bbX 3991 bbX 9 bb 447 bb 415 bb 219 m 418 bb 434 Ml 1775 bb 19 MM 46 bb 95 MM 212 bb 422 bb 19 bb 1818 bb 3158 bbX 4081 bbX 0.85 3.69 10.39 24.79 48.04 99.6S 240.63 407.36 541.42 0.00 59.33 55.07 28.36 -IS -26 -1 -4 -0 -4 -19 -28 13 55.45 57.55 240.01 -4 1.10 4.76 11.48 27.42 56.00 109.94 245.90 428.05 553.60 10 -5 15 9 12 10 -2 -15 -26 Soup 020199: Quantitatad and printad by iaa on 10/29/99 Quantify C c ^ e u n d Itaaaiy tepore 0 X1 4 5 -twann 16 doa< eoftiizaktloa* f f O i / > P 0 t t / M U at 10/20/99 is List: C:\lttBSLWX\aoup020199.proV8nWlnBB\10a89J teat nodltiad: rri Oct 29 07:02:5 1999 tetbed: C:\MteStnB\aoup020199.pcoVMOt&n\10a99 teat aodlflad: fri Oct 29 0(:5):SS 1999 Job Coda: Pritad: Pri Oct 29 07:37:25 1999 2: PPO (Cfc2) 1 102899001 2 102899002 3 102899003 4 102899004 5 102899005 102899004 7 102899007 8 102899008 9 102899009 10 102899010 11 102899011 12 102899012 13 102899013 14 102899014 15 102899015 16 102899016 17 102899017 18 102899018 19 102899019 20 102899020 21 102899021 22 102899022 23 102899023 24 102899024 25 102899025 26 102899026 27 102899027 28 102899028 29 102899029 aaplaliat Tant MaOH Blk MaOH Blk PQtix-99086-43-1, Ippb- 9/10/99 BMW POJC-990S6-43-2. 5ppb- 9/10/99 BMW PCMijr-99086-43-3. lOppb- 9/10/99 BMW rCMix-99086'43-4. 25ppb- 9/10/99 BMW rCKix-99086-43-5. 50ppb- 9/10/99 BMW lOOppb- 9/10/99 BMW 250ppb- 9/10/99 BMW 500ppb- 9/10/99 BMW 750ppb- 9/10/99 BMW MaOH Blk TOX145-PPOS/POAA in Tvaan-doaa-2ppb- 10/28/99 ZAS TOX145-PPOS/POAA in Twann-e-4ppb- 10/28/99 IAS fCMix-99086-43-4, 25ppb- 9/10/99 BMW MaOH Blk TOX145-PPOSA in Twaan-doaa*200ppb- 10/28/99 IAS wen-a>300ppb- 10/28/99 ZAS 250ppb- 9/10/99 BMW Type Standard Standard Standard Standard Standard Standard Standard Standard Standard QC lppb- 9/10/99 BMW Sppb- 9/10/99 BMW lOppb- 9/10/99 BMW 25ppb- 9/10/99 BMW 50ppb- 9/10/99 BMW lOOppb- 9/10/99 BMW 250ppb- 9/10/99 RWW 500ppb- 9/10/99 BMW 750ppb- 9/10/99 BMW Standard Standard Standard Standard Standard Standard Standard Standard Standard Btd cone 1.01 5.03 10.00 25.20 50.30 101.00 252.00 503.00 755.00 252.00 1.01 S.03 10.00 25.20 50.30 101.00 252.00 503.00 - 755.00 RT 7.248 7.265 7.226 7.268 7.247 7.248 7.254 7.247 7.272 7.287 7.290 7.289 7.291 7.287 7.291 7.294 7.273 7.267 7.294 7.288 7.288 7.287 7.268 7.295 7.286 7.291 7.295 7.289 7.266 a t m nap* 95 MM 53 MM 109 bb 442 bb 905 bb 2086 bb 4177 bb 8256 bb 21703 bb 39235 bbX 54526 bbX 167 bb 29376 bb 30229 bb 2326 bb 55 Ml 30004 bb 29852 bb 22582 bb 88 bb 141 bb 514 bb 987 bb 2248 bb 4459 bd 8735 bb 22119 bd 38876 bbX 53247 bbX Cone. 0.63 0.14 0.79 4.67 10.07 23.83 48.19 95.72 252.39 456.65 634.82 1.47 341.79 351.73 26.62 0.16 349.11 347.34 262.63 0.54 1.17 5.51 11.02 25.71 51.47 101.29 257.24 452.47 619.91 -21 -7 1 -5 -4 -5 0 -9 -16 6 4 16 10 10 2 2 0 2 -10 -18 Pae* 2 Soup 020199: Quteticatad and printed by i u on 10/29/99 O u M t i f y Cawpcraiut m i r y I l O X l O ' t v M n 0 dosa confi: prOS/PFOSA/POAA m e . 1 6 / 2 9 / 9 9 ill 1 ^ 1 use: C:\MA88MKX\teup030iS9.pro\8teplaM\102499a b u t tedifid: H i Oct 3 07:03:5 3559 Hotted: C:\KM0UnBVMUp030199.prO\mebBB\10aa9* tese aodiflod: rrl Oct 29 04:53:35 1999 Job Cod: Printed: rrl Oct 29 07:37:35 1999 **--- r**" - * 3: r r o u (Chi) 1 102899001 2 102899002 3 102899003 4 102899004 5 102899005 6 102899006 7 102899007 8 102899008 9 102899009 10 102899010 11 102899011 12 102899012 13 102899013 14 102899014 15 102899015 16 102899016 17 102899017 18 102899018 19 102899019 20 102899020 21 102899021 22 102899022 23 102899023 24 102899024 25 102899025 26 102899026 27 102899027 28 102899028 29 102899029 Steplsliat Taxe M0H Blk M O H Blk FCHix-99066-43-1. lppb- 9/10/99 RMW ratix-99086-43-2. 5ppb- 9/10/99 RMW FOlix-99086-43-3, lOppb- 9/10/99 RMW PCHix-99086-43-4, 25ppb- 9/10/99 BMW PQtix-99086-43-5, SOppb- 9/10/99 BMW PCHix-99066-43-6. lOOppb- 9/10/99 BMW POtix-99086-43-7, 2S0ppb- 9/10/99 RMW FQiix-99086-43-8. 500ppb- 9/10/99 RMW FOti*-9908 6-43-9. 7S0ppb- 9/10/99 RMW HOH 81k TOX14S-PrOS/POAA la TWtea-de-2ppb- 10/38/99 IA5 TOX145-PFOS/PQA la Twa-M-4ppb- 10/28/99 IAS PQlix-99086-43-4, 25ppb- 9/10/99 BMW M0H Blk TOX145-PPOSA la TV*n-dosf200ppb- 10/28/99 IAS TOX145-PPO&A la Tv*n-S-300ppb- 10/28/99 XAS POtix-99086-43-7, 250ppb- 9/10/99 RMW MaOR Blk POlix-99086-43-1. lppb- 9/10/99 RMW PQIix-99086-43-2. Sppb- 9/10/99 RMW PQijjc-99086-43-3, lOppb- 9/10/99 RMW POtix-99086-43-4. 25ppb- 9/10/99 BMW POtix-99086-43-5. SOppb- 9/10/99 BMW PCHix-99086-43-6. lOOppb- 9/10/99 BMW POtix-99086-43-7, 2S0ppb- 9/10/99 BMW FQCix-99086-43-8, SOOppb- 9/10/99 BMW FCHix-99086-43-9. 750ppb- 9/10/99 RMW Typ Standard Standard Standard Standard Standard Standard Standard Standard Standard QC QC Standard Standard Standard Standard Standard Standard Standard Standard Standard td Gene 1.01 5.03 10.10 25.10 50.30 101.00 251.00 503.00 754.00 25.10 251.00 1.01 5.03 10.10 25.10 50.30 101.00 251.00 503.00 . 754.00 RT 7.811 7.802 7.766 7.786 7.764 7.765 7.771 7.765 7.811 7.826 7.831 7.829 7.853 7.849 7.831 7.856 7.835 7.852 7.833 7.829 7.851 7.828 7.829 7.836 7.823 7.831 7.830 7.830 7.808 A T M Flaps Cone. U l T 559 db 0.00 204 KM 0.00 762 MKX 0.00 -100 2539 bbX 0.00 -100 4612 MKX 2.11 -79 10800 MM 17.23 -31 19708 bb 39.00 -22 43375 bb 96.84 -4 105704 bb 249.16 -1 205809 bb 493.80 -2 301294 bb 727.16 -4 2511 Mt 0.00 4283752 bb 4315922 bb 10459.75 10538.37 63186 MK 145.25 479 12460 MM 21.29 4302369 bb 10505.25 4271995 bb 10431.02 159170 MM 379.83 51 14836 IM 27.09 8217 MKX 10.92 961 8161 KMX 10.78 114 9260 MKX 13.46 33 16554 bb 31.29 25 25954 bb 51871 bb 54.26 6 117.60 16 120810 bb 286.08 14 217005 bb 521.17 4 304590 bb 735.21 -2 Soup 020199: Quaatltatod ad printed by 1 on 10/39/99 ti m i T Lise : Cs MOSSUriCXNaonpOZOm .pro\a*laI*\203B99 L M t wdiflad: Fri Oct 29 07)02*56 1999 Wtbed: C:\ML99Z.TKX\aoup020199.proNM*CbOaM02999a U a t dlfttd: Fri Oet 29 0(sUt)S 1999 Job Cod*: Printed: Fri Oet 29 07:37*25 1999 Oeapound 4: Z9 (Cb4) 1 102899001 2 102899002 3 102899003 4 102899004 5 102899005 6 102899006 7 102899007 8 102899008 9 102899009 10 102899010 11 102899011 12 102899012 13 102899013 14 102899014 15 102899015 16 102899016 17 102899017 18 102899018 19 102899019 20 102899020 21 102899021 22 102899022 23 102899023 24 102899024 25 102899025 26 102899026 27 102899027 28 102899028 29 102899029 lanplellat T M t H*OH Blk HeOB Bit POJC-990S6-43-1. lppb- 9/10/99 K M FQJC-99086-43-2. Sppb- 9/10/99 K M rQJt-99086-43-3, lOppb- 9/10/99 W W FQlix-99086-43-4. 2Sppb- 9/10/99 K M FOHx-99086-43-5, 50ppb- 9/10/99 K M FCXix-99086-43-6, lOOppb- 9/10/99 K M FQIjc-99086-43-7, 250ppb- 9/10/99 K M FQLix-99086-43-8, SOOppb- 9/10/99 K M rOtin-99086-43-9, 7S0ppb- 9/10/99 K M OH Blk TOX14S-PPOS/FQAA in Teeen-doa#-2ppb- 10/28/99 XAS TOX145-PPOS/FQAA in Tween-na-4ppb- 10/28/99 XAS FQtix-99086-43-4, 25ppb- 9/10/99 K M TQ214S-PPOSA in Teen-do**-200ppb- 10/28/99 ZAS TOX14S-PFOSA in tveen-na-300ppb- 10/28/99 IAS FOx-95086-43-7, 250ppb- 9/10/99 K M HeOB Blk Ftaiix-99086-43-1. lppb- 9/10/99 K M FQIix-99086-43-2, Sppb- 9/10/99 K M FCHix-99086-43-3. lOppb- 9/10/99 K M FOtix-99086-43-4, 2Sppb- 9/10/99 K M FCXix-99086-43-5. SOppb- 9/10/99 K M POtin-99096-43-6. lOOppb- 9/10/99 K M POlix-99086-43-7, 2S0ppb- 9/10/99 K M FCKix-99086-43-8. SOOppb- 9/10/99 K M PCMix-99086-43-9. 750ppb- 9/10/99 K M Typ* Standard Standard Standard Standard Standard Standard Standard Standard Standard OC OC Standard Standard Standard Standard Standard Standard standard Standard Standard .Cene ta 7.081 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 7.083 7.102 7.101 7.103 7.109 7.102 7.105 7.120 7.124 1.00 7.124 7.120 7.124 1.00 7.128 7.124 7.127 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 7.145 7.143 7.125 7.151 7.141 7.147 7.149 7.145 7.121 Area rlapa 16 bb 4165 bb 4646 bd 4643 bb 4814 bb 4546 bb 4172 bb 2878 bd 2479 bb 2203 bb 3463 k*> 3528 bb 3185 bb 3679 bb 3545 bb 2681 bb 3119 bb 3041 bb 2979 bb 2937 bb 2907 bb 2907 bb 259S bb 2441 bb 2112 bb Cane. Drr 0.00 -100 1.26 1.40 1.40 1.45 1.37 1.26 0.87 0.75 0.67 26 40 40 45 37 26 -13 -25 -33 1.05 1.07 0.96 5 7 >4 1.11 11 1.07 7 0.81 -19 0.94 0.92 0.90 0.89 0.88 0.88 0.78 0.74 0.64 -6 -8 -10 -11 -12 -12 -22 26 -36 Soup 020199: Quantitated and printed by ina a 10/29/99 T * * - I * / Tl U t J- U H * 9MQ9 1 oup 020199; Quantitt* tad prit* br l* 10/39/99 Quantity Calibrati -- port , i a U 4 5 - t -- 0 -- o o o f l n t i - FTO/FFO-- /o-- t . 10/2/ in* -- up 020199> Quantitatad and printad by ina 10/29/99 o* 2 XX Soup 0201*9 : QuMtiiaead ad prlatad by Im 1 0 /2 9 /9 9 Quantify Calibration Mp o r t Y0S14S-twaaa 0 4oaa ooofi*nationi- rroa/rroaJk/Q&Jk axe. 10/3*/ U i Compound 4 name: IS (Ch4) Response Factor: 3310.11 Response type: External Std, Area Curve type: RF 4.81 e3-i x x X X X xxo< oop 03019ft Quanticatad and printad by laa on 10/39/99 -' ' ., ~ '*" " Method (lepore Matbod Cile: Last Modified : Compound: Printed: C:\MASSLYHX\edup020199.proNMetbDB\102899a.mdb Fri Oct 29 OC:S3 :35 1999 1: PGAA (Chi) Fri Oct 29 07:31:25 1999 COMpound Neste: Internal Ref.: Quantify Trace: Cone, of Standards: User RF Value: Vacr Peak Factor: Integrate Window Factor: Chromatogram mass window: FQAA (Oil) (Mo m ] TIC Cone. A 1.000000, Disabled 1.000000 2.000 l.OOOODa Retention Tie (ains): Relative Retention Tima: RT Reference: Tine Window (mine): Peak Selection: 7.152. Enabled 0.000, Disabled (Mo m ] 0.356 Nearest Response Type: Response: Bxternsl Areas Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Linear Exclude 1/X Units: Peek-to-peak amplitude: Smoothing: Window site {scans): Number of smooths: Smoothing method: 63 Enabled 2 1 Join valley threshold: Reduce peak tailing: Raise baseline maximum: 30.00 200.00 5.00 Draw vertical threshold: Detect shoulders: Shoulder threshold: 90.00 Disabled 30.00 ` Relative height: Absolute height: Relative area: Absolute area: 1.50, Diaabled 0.00, Disabled 2.00. Disabled 0.00, Disabled 1 m* / ____ Feg 1 Method Report Method file: Leet modified: Comound: Printed: C:\KRSSLYMX\aoup020199 .pro\MethDEU02l99a.mdb rri Oct 2 06:53:35 1999 2: PTOS (Ch2) fri Oct 29 07:31:25 1999 Compound Name Internal Ref.: Quantify Trace: Cone, of Standard: User RP Value: User Peak Factor: Integrate Window Factor: Chromatogram mass window: pros (Ch2) (Monel TIC Cone. B 1.000000, Disabled 1.000000 2.000 l.OOOODa Retention Time (mins): Relative Retention Time: RT Reference: Time Window (mins) : Peak Selection: 7.335. Enabled 0.000, Disabled (Monel 0.334 Heareat Response Type: Response: External Areas Polynomial Type: Point of Origin: Pit Weighting: Axis Transformation: Linear Exclude 1/X None Units: Peak-to-peak amplitude: Smoothing: Window sise (scans}: Humber of smooths: Smoothing method: Join valley threshold: Reduce peak tailing: Raise baseline maximum: Draw vertical threshold: Detect shoulders: Shoulder threshold: Relative height: Absolute height: Relative area: Absolute area: IS Enabled 2 1 30.00 200.00 5.00 90.00 Disabled 30.00 . 1.50. Disabled 0.00. Disabled 2.00. Disabled 0.00. Disabled dethod Report Method file: Last modifisd: Compound: Printed: C:\KASSLYMX\soup020199 .pro\KsthD8\102899a.mdb Fri Oct 29 08:52:25 1999 2: PFOSA (Chi) Fri Oct 29 07:28:25 1999 Compound Na m : Intarmi Rat.: Quantify Traa: Cene, of Standards: Osar RP Value: Usar Peak Factor: Integrata window Pactor: Chromatogram mass window: RPOSA (Chi) [Bone] TIC Cene. C 1.000000, Disabled 1.000000 2 .0 0 0 l.OOOODa Retention Time (mins): Relative Retention Time: RT Reference: Tima Window (mins) : Peak Selection: 8.052. enabled 0.000. Disabled [None] 0.4*5 dearest Response Type: Response: External Areas Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Linear txclude 1/X dona Units : peak-to-peak amplitude: Smoothing: Window size (scans): dumber of smooths: Smoothing method: Join valley threshold: Reduce peak tailing: Raise Vaseline maximum: Draw vertical threshold: Detect shoulders: Shoulder threshold: Relative height: Absolute height: Relative area: Absolute area: 147 Enabled 2 1 20.00 200.00 5.00 90.00 Disabled 20.00 1.50, Disabled 0.00, Disabled 2.00. Disabled 0.00, Disabled , Page 2 Method Report Method file: Leet modified: Compound: Printed: C:\MASSLY1Ct\soup02Q199.pro\MethDB\102l99e.mdb Fri Oct 29 06:53:35 1999 4: IS (Chi) Fri Oct 29 07:30:25 1999 Compound Neste: Internel Ref.: Quantify Trees: Cone, of Standerds: Doer RF Velue: User Peek Factor: Integrate Window Factor: Chromatogram mess window: IS (Chi) (Mono) TIC Fixed 1.000000. Disabled 1.000000 2.000 l.OOOOOe Retention Time (suns): Relative Retention Time: RT Reference: Time window (mins): Peak Selection: Response Type: Response: 7.190. enabled 0.000. Disabled (Mona! 0.290 nearest external Areas Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Linear Exclude 1/1 one Units: Peak-to-peak amplitude: Smoothing: Window size (scans): Humber of smooths: Smoothing method: Join valley threshold: Reduce peak tailing: Raise baseline sttxinm: 70 Enabled 2 1 30.00 200.00 S.OO Draw vertical threshold: Detect shoulders: Shoulder threshold: 90.00 Disabled 30.00 * Relative height: Absolute height: Relative area: Absolute area: 1.50. Disabled 0.00, Disabled 2.00. Disabled 0.00, Disabled Peg* 4 H * * /? ? /y > ^ Quattro II, #6414E SOUP 020199: FACT Equipment Log 99092 PAGE 1/1 DATE: 10-28-99 ANALYSTMas . STUDY NUMBER:TOX145 MATRIX: Tween samples DESCRIPTION: d(?se confirmation FACT Method: Injection volume- 10 uL Cycle time: 10 min. Electrode: Z-Spray-------- Mobile Phase: (A12.0 mM NH4CH3CQ2 (B) McOH-------- TN-A- or stndrd number (A) 99085-11-3________ (B) TN-A-299?_ Prepared (date/by): (Ai 10/21/99 mmh_______ (B) IQ/10/99 sab Expires: (Ai 04/00_____________ (B) 2010--------- Store at room temp? [Yj or N Other:-------- -------------------------- Guard column: None__________ ______ Part number: na__________ Lot number: na Analytical column: Keystone Betasil ______________________________ Size: 2 x 5 0 mm_______________ Type:_Q8__________ Sphere size:JLum--------Part numher 055-701-2_________ Lot number: P9E11 Serial numbcr:05918047 Analytical parameters: Drying gas (L/hrl: 350 ESI nebulizing gas (L/hrl 13 LC Flow rate: 300 uL/min. Back pressure: 65 bar Sheath gas (L/hr)_0 HPLC solvent gradient: 10min-10-95 Tim e (m in.l_____ 1 1 0 . 0 0 ____________ 21 1.00________ 3) ^ 5 0 _________ 4) i 5 0 _____ 518.00_________ %B 10-0 10.0 _2M. 21Q_ 10.0 T u n in g M ethod R e p o rt Method: C:\MASSLYNX\SOUP020199.PR0\ACQUDB\PF0S3 Printed: Thu Oct 28 15:21:34 1999 /0 /jL fJ < )9 Page 1 SOURCE ( ESP - ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. Set Rdbk 1.60 60 5 0.2 150 250 1.59 -60 -7 153 249 P ressu res Analyser Vacuum Gas Cell Rdbk 6.le-5 4.le-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set 14.0 14.0 0.9 0.0 4 650 S e t Rdbk 14.0 14.0 60 2.0 0.0 40 0 650 28 38 28 Method Report itothod Filet I*aat M o d i f i e d : Printed C t \MXaSLYHX\SOUF020199 .PROYJLCQUDB\10mIi-10-95 Thursday Oct o b e r 28/ 1999 13t44i34 Thursday/ October 28/ 1999 13>44s44 KP1100 LC Pump Initial condition* Solvents A% B% C% D% 90.0 10.0 0.0 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 0.300 10.0 0 400 30.0 30.0 HP1100 LC Punp gradient Timetable The gradient Timetable contains 5 entries which are : Time 0.00 1.00 5.50 7.50 8.00 A% 90.0 90.0 5.0 5.0 90.0 B% 10.0 10.0 95.0 95.0 10.0 C% 0.0 0.0 0.0 0.0 0.0 D% 0.0 0.0 0.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 HP1100 LC Pump external Crant Timetable The Timetable contains 3 entries which are : Time Initial 0.00 0.10 Column Switch Contactl Off Off Off On Off Off Contact2 Off On Off Contact3 Off Off Off Contact4 Off On Off SP1100 Antoaamplar Initial Condition* Draw Speed Eject Speed (pl/min) Draw Position (mm) Stop Time (mins) Injection Volume(pi) Vial Number 200.0 200 0.00 9.00 10.0 41 /H & c r Pag* 1 Pressure 400 400 400 400 400 MKho4: L U C IBdltUd: Srlstad: c\llMLTl\K)OM0H.D\JinM<MI-FFO-O-FI-I rrt Oct IS UiSSiOS I S M m Oct as 131*1:1 1SSS Solvent Dalay ( nina ) t 0.00 Function i 1 M M of 1 Maas Fair ( ESP- ) Zator Channel Delay ( Secs ) : Span ( Daltona ) : Stare Tina ( Nioa ) : End Tina ( Miaa ) : Repeats ; Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Sees) Coll Energy (eV) 1 411.00 149.00 0.30 30 Cone ( V IS Function < 2 M M of 1 Maas Fair ( MSP- ) Inter Channel Delay ( Secs ) i Span ( Daltons ) : Start Tina ( Kins ) : End Tina ( Mins ) : Repasts : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) Cell Energy (eV) 1 499.00 99.00 0.30 4S Cone ( V 40 Function i 3 M M of 1 M u i Fair I W - ) Inter Channel Delay ( Sees ) : Span ( Daltona ) : Start Tine { Mins ) : Bad Tine ( Mins ) : Repeats s Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) Coll Energy (eV) 1 498.00 78.00 0.30 45 Cone ( V 40 Function : 4 MEM of 1 Mans Fair ( MSP- ) Inter Channel Delay ( Sacs ) : Span ( Daltona ) : Start Tina ( Mina ) : End Tine ( Kina ) : Repeats : Channal Paxant Daugbtar 0.03 0.00 0.00 10.00 1 Dwell (Secs) Coll Energy (eV) 1 427.00 80.00 0.30 40. Cone ( V 40 i^ /9 ? /n e z r Masslynx - Sample List Sample List: C:\MASSLYNX\soup020199.pro\SampleDB\102899a.SPL Printed: Thu Oct 28 13:44:09 1999 tM s/9 9 /n & r Page 1 Page Position: (1,1) File Name File Text MS File 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 102899001 102899002 102899003 102899004 102899005 102899006 102899007 102899008 102899009 102899010 102899011 102899012 102899013 102899014 102899015 102899016 102899017 102899018 102899019 102899020 102899021 102899022 102899023 102899024 102899025 102899026 102899027 102899028 102899029 MeOH Blk MeOH Blk FCMix-99086-43-1, 1ppb- 9/10/99 RWW FCMix-99086-43-2, 5ppb- 9/10/99 RWW FCMix-99086-43-3, 10ppb- 9/10/99 RWW FCMix-99086-43-4, 25ppb- 9/10/99 RWW FCMix-99086-43-5,50ppb- 9/10/99 RWW FCMix-99086-43-6,100ppb- 9/10/99 RWW FCMix-99086-43-7,250ppb- 9/10/99 RWW FCMix-99086-43-8, 500ppb- 9/10/99 RWW FCMix-99086-43-9, 750ppb- 9/10/99 RWW MeOH Blk ,, T O X 145-PFOS/POAA in Tween-dose-2ppb- 10/2S/99 IAS TOX145-PFOS/POAA in Tween-ms-4ppb-10/28/99 IAS FCMix-99086-43-4, 25ppb- 9/10/99 RWW TOX145-PFOSA in Tween-dose-200ppb-10/28/99 IAS TOX145-PFOSA in Tween-ms-300ppb-10/28/99 IAS FCMix-99086-43-7, 250ppb- 9/10/99 RWW MeOH Blk FCMix-99086-43-1,1ppb- 9/10/99 RWW FCMix-99086-43-2, 5ppb- 9/10/99 RWW FCMix-99086-43-3,10ppb- 9/10/99 RWW FCMix-99086-43-4, 25ppb- 9/10/99 RWW FCMix-99086-43-5, 50ppb- 9/10/99 RWW FCMix-99086-43-6,100ppb- 9/10/99 RWW FCMix-99086-43-7,250ppb- 9/10/99 RWW FCMix-99086-43-8, 500ppb- 9/10/99 RWW FCMix-99086-43-9,750ppb- 9/10/99 RWW 10 M IN -P F O S -P O A A -P F O S A -IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10 M IN -P F O S -P O A A -P F O S A -IS 10MIN-PFOS-POAA-PFOSA-IS 10 M IN -P F O S -P O A A -P F O S A -IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10 M IN -P F O S -P O A A -P F O S A -IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS Masslynx Sample List Sample Ust: C:\MASSLYNX\soup020199.pro\SampleDB\102899a.SPL Printed: Thu Oct 28 13:44:09 1999 Inlet File Bottle Inject Volume Sample Type Cone A ConcB ConcC 1 10min-10-95 91 2 10min-10-95 91 3 10min-10-95 1 4 10min-10-95 2 S 10min-10-95 3 6 10min-10-95 4 7 10min-10-95 5 8 10min-10-95 6 9 10min-10-95 7 10 10min-10-95 8 11 10min-10-95 9 12 10min-10-95 92 13 10min-10-95 10 14 10mirv-10-95. 11 15 10min-10-95 4 16 10min-10-95 92 17 10min-10-95 12 18 10min-10-95 13 19 10min-10-95 7 20 10min-10-95 92 21 10min-10-95 1 22 10min-10-95 2 23 10min-10-95 3 24 10min-10-95 4 25 10min-10-95 5 26 10min-10-95 6 27 10min-10-95 7 28 10min-10-95 8 29 10min-10-95 9 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 --- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- / /> rjy y Page 2 Page Position: (2,1) FACT: DATA REVIEW SUMMARY FORM Data Analyst: FACT Study ) : sk JS Mstnx/Timcpoints: Sample t ' - Cor>(j j f / f f Set-up Analysis Date/Analyst: nstniment 3** " k h i * J . 02</9* ___JbA (ao) Acceptable Linear Range: LOQ:.. /.? g 0U Y R"2: /-3 o r * l JL Y ft* - 7 7 Extraction Blank: "i/SS n VXiUa. //>0 Matrix Blank: J s _ /La. U q Calibration Checks: OK - h * . -5~^---- > -/0^ MS/MSD: K)|fV-_________________ ___ ________ Data Status; -D frffr M rf Aa,|y,:- 7 fc s CCHl'O - yudJ abbi Acceptable Linear Range: LOQ: RA2: J 2 - o ^ l?... 0-1?ZM1 Calibration Checks: fe-S o jd , y Extracted Blank: Lss 41*+.qn Matrix Blank '/La a IoQ -? ? > ------ ? ~ /3 'l M S ^ I S P 7 t% , Data Status: xyfA'ii 0 J 4 f/^iU.Enrico Analyte: Stu-r ff3' ) " Acceptable Linear Range: AM LO Q :______ AM R'2: -/A . Calibration Checks: MS/MSD: /V/zfr _A2L DaUSatur. g fc -fltl a I/Ift Extracted Blank ^/A Matrix Blank aM- D ata Review Sign-O fT Analyst Review Name / Date: "Ia s N ^ e " / ^ ^ ^ ,, ! via * j f a { ( { f f a f Quality Assurance Review N am e/D ate: Data E ntry:___ C W ls W S j$ / Comments/ Justifications: Q W 5>"/*V y ^ Uu i t IS - L . B m U . -4 \_IlJ- Z< Kk L s -Aa^ ILaJc ; ~)U 7* llM n ext/ u j i c / -fn tu . J L r * n j* -L ' dt& tka.fiC j (L dhjg_ p z\l a ^G sC -t/hbaJt '- M L < L y c Jo eg** SSiicGftild C id L /r/TcJe/h ___ -L i h r}U ,fl.rf /nA r/s t i r / <d h t OHa7J ^jL 'fref/p -y ___________________ ____________ ___ O b y / i d J V 'J - U f y A tu ts ,,_J. _ Z * i j h r -JU ^ L /^ .l' J d p * d la x -exc/uJ t J J u j / s J t f d d __ a- d / i t Shyu ~ a w H a tte a. 4b7 4 U J f -- TV- t/r. L ~ . * * s uf i t h i d J iL O fjt.L L _______________ / JLL Cu.* /z z r l 2? jw d e a. L v 7n />(. d ld c c j d b fu'!/Lints- K tttC fi aa T^ irr oo ^ n a b ^ d L ,- X s Q S fJ a.^en. oiL^JSi Ui _ a !l e*J r / Sa. ^ L s n d 4 L . JUs /mls* L ui. - J2rS *U j * , ____________ ^ i* b i f - FACT: DATA REVIEW SUMMARY FORM Date Data Analyst' 3 5 FACT Study#: 7 ox/Y 5 Matnx/Timepoints: Ib J -b ik r -C a d ra i f JoSe. Jea 29 - Sample List 1 Set-up Analysis Date/Analyst `'/i- b D ata Review Sign-O fT Analyst Review . Name / Date: H** Technical Review . Name/Date: A tr i ) ocm^ 1 I i5 Quality Assurance Review Name /Date: /A C / i / 0i / w Data Entry: f t -t^r nag*. 1 -...lAC n / t f h l r ? e i i i i i ? % s I s isS siss s ssg 32555200000 SOO SdESSriggggg Sgg ggggggf gSg ggg I s s s s s 2 s s 2 2 i ; s 5 5 i i s s g,,0000SOOOSS StSSSSooOOO gggggg ggggri Sg5523g gggg gggggg gggggg gggggg^ggg t f P 3 < ! 3 'fw 222222i2222222222ii2222222S2222222222222 jMgg.sggggs;?sssssgssgggsggg^3??gss;ggs si;:s SoooooosS3S s2ss0=r oo000Ss30ss2 S 5 :h 3SS |^*=SSSSi5iS3=S|=gg-SSp=|||=S=S|||| S Sg3:23= S3P 5:32S?SS3SSE E E P 3?S3K S3 SSSS8SSSS :sgsggggg " sssassag SH a = - -- s n lll *! ~ 3 P 1 1 1 1 1 1 a i l i l i a i , afflli IM!ti! s lili!! il _ m m m m m m m itSSSiggiBggeiSgggSBgiSiiei l "233: ;22S3323SS2SaS323S333SSS;33; 8 m jf ? 2to S a I 1 f es i E ? i ? % sssssssss s s s sss'ss's's's's 9t J J -J s j <j >j vj i i s i i s s i s i s S i i 5S S g g i s S S g s s i m m m m igii 3 >- O "'OC ; S S S S 2 i : 3 2 S 22 SZSZZ S S K S S g S S g S S S S S S ggggggggggg ggg gg ggg gggggggggggggggggg i uiwkooHH -js-j * *o*o'Si>l' IMii 'j MMJ r J MKl MkJMM * U Kl M O W O ~ o o o o o o o o o oo oo oo oo oo o o o o o o o o o o o o o o o o o o o o o oooo o oo !. . ui(k ui u u> it tr wwwwwwwww o o o o o o o o o o o o o o o o o o o o o"o oO O O O O O O O O O O O O O_ . 0 0 0 0 0 0 0 000000000 I nm n i I n ? ?? ggggggggggggggggggggggggggggggggsgggggggggggl i/tfV M uvvv>vu<u itP U 'tfU 'aiu < v iu < v u 'V iH v iv v < v v > u '9 u tu > u iu iu iu iu iu iu ig ii> ig t0 ii^ siissiiiiihhshhhiihhhhhkisH issksski C E E E E E E E M E ,irM r ,r ,rE r r r r r ' * ,E r r ,r r ,r " 'n E i - j E C r`M E E E * * * * 00000000000 * * * * * A A ik * * * O O WWWWW O * 0 O O O O O O O O O O O * j g V 58 58 58 59 58 A 58 58 58 58 58 * K i . * < i K i i * * * 000W 000 >* * <<* <11( 1 W O O W O O O O O W O O O O O WW<0WW<PWW<0WW I UU I UUUUU UUUUU I I I I I I I I I t I MPPUHPWHPSI UNN WKIMKIMW WNMMNN H0 UO8 W 9 N O O O M O Kl W BB V O 1 / 8 O U> W< U> * * O * <0 * * 0 N O O O K / O O K / ' O t o -qddO l S55 555555 55??? SSSS?7TS * 5 5 *5 5 5 5 5 * l l l s s f * * * ? T?*? . r r r - f AS? A????? S S S v v ? r r r - r f * ' , , - ~ i s s s s * * D'as's l i r ,,r 3 3 3 ? , ? 55 55555 555 , 5 1 5 5 3 3 3 ? ? 51?~?~??_S1?S1fi' -2!'-8 5**if |f ijariBaSa ' >S1P9S9S'? 3I? ? ? ?, >,>'), 3l-i -SSSSSSS"-" 3 , fSSSi .?i?S5Sl" - OX K M K K W W W WW X5 WW 1 9 * 1 9* O- O- I O O- O-h-*"ns.ft> OXK K M M w w w wW xO wW WWWWWWWI I V B B ' P S WWWWWWWI I WW WJ J W IW IWK)I WI I Wf t H/ W NH OX ft- f<t-- * fmt- fft-- fftt-- ft- ft- X0 H H H 0 *0v w VWC WI WI W| W| NI I fI JKMI WH f0t fHt 1 MMNNHHHH ! H VS SSSH M !--- -- kJH H HH H H H HHHHH M W* P H SS 0PPA SS 0SSS W SS S P P 0 * * *BB Mf t - f t - f t - f t - f t - f t - f t - K> ft- ft. ft^ ft* -> ft. " H I 00 I 0 0 0 S S ISS S 6 H ft- WWW M W W W W W M W W W X K - ft- W W ft- W W W *- ft- >- W w ww E ft I I MMMMHHHH | M r*rrr*r*rr*rft sssssssss im llm *1 *1 h *i J0 <UM JNHo wfl Jouguk j w j -J / . jgwggg. / g g g g g 1. I 8O g f* t UU gt >o M0 *-Hft-8 k l H 0 M ftH U M 0t 0* Kft-ft OMNK)H V g00gNH0NKk*M M0OI O0 0 #1HH 0MHHWU *UOU*KI9NHHH kiwh Hkj8ft0g000ftu0ftg0wggwuuuftuft8ig>*ftMO0ftMNg8000p0ui f t H f t k j 0 M 0 y H H 0 H u u K j 0 M M t g 0 i - > f t g N * N i M M g 0 8 i H g i g 0 H K < 0 Uik>9 3 1 Quantify Calibration Raport TOXJ45-rat livor, Day29 doao and control- oat. 11/4/ to n Compound 1 name: POAA (Chi) Coefficient of Detennination: 0.989198 .Calibration curve: 0.973462 * x + 119.913 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None J i* ulo x h ( > / - / H Pa9 1 Analla 062491: Quantitated and reviewed by iaa on 11/1/99 Quantify Calibration Report TQX14S-rat liver, Day?9 dose and control- cat. 11/4/99 W W Compound 2 name: PFOS (Chi) Coefficient of Determination: 0.982749 Calibration curve: 9.51640 * x + 260.801 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None 9*9 2 Aaella 0(249: Quantitated and reviewed by ias on 11/8/99 Quantify Calibration Report .. ... . TOX14S-rat livor, Day29 4o m and control' oat. 11/4/ 1 Compound 3 name: Sun (Chi) Response Factor: 4773.57 Response type: External Std, Area Curve type: RF Pago 3 -18.5 Cone 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 Aaalia 042498: Quantitated and rovlovod by laa on 11/8/99 Quantify Calibration noport TOX145-rat livar, Day2 do* and itrol- ost. 11/4/M M W Compound 4 name: PFOSA (Ch4) Coefficient of Determination: 0.989845 Calibrationcurve: 17.2655 *x+131.101 Response type: External Std, Area A . VT Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None Am II* 0C2499: Quantltatod and ravlavad by laa on 11/9/99 Metnod Report Method file: Last Modified: Coapound: Printed: r : \ i H l u backup sep99\aelia-rata.pro\MathDB\110599a.imdb Mon Nov 01 08:20:27 1999G 1: PQAA (Oil) Mon Nov 01 08:56:38 1999 Coapound Nan*: Internal Ref.: Quantify Trace: Cone, of Standards: User RF Value: User Peak Factor: Integrate Window Factor: Chromatogram aass window: Peak Location Retention Tine tains!: Relative Retention Tiae: RT Reference: Tiae Window tains): Peak Selection: Response Response Type: Response: Calibration Curves Polynoaial Type: Point of origin: Fit Weighting: Axis Transformation: Concentration Units: Noise Peak-to-peak amplitude: Smooth Smoothing: Window size (scans!: Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: Peak Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative area: Absolute area: PORA (Chi) (Nona] TIC Cone. A 1.000000, Disabled 1.000000 2.000 1.00000a 6.976, Enabled 0.000, Disabled [Nonal 0.274 Nearest External Areas Linear Exclude 1/X None ' 530 Enabled 2 1 30.00 200.00 S.00 90.00 Disabled 30.00 . 1.SO, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled Peg l Method Report Method file: Lest Modified: Compound: Printed: r:\amelia backup sep99\ameliaMon Nov 0 08:20:27 1999C 2: Pros (Ch2! Mon Nov 08 08:58:38 1999 Compound Name: Internal Ref.: Quantify Trace: Cone, of Standards: User RF Value: User Peak Factor: Integrate window Factor: Chromatogram mass window: Peak Location Retention Time (mins): Relative Retention Time: RT Reference: Time Window (mins): Peak Selection: Response Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Concentration Units: Noise Peak-CO-peek amplitude: Smooth Smoothing: Window size (scans): Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: Peak Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative area: Absolute area: pros <Ch2) (None) TIC Cone. B 1.000000, Disabled 1.000000 2 .0 0 0 l.OOOODa 7.149, Enabled 0.000, Disabled [None] 0.299 Nearest External Areas Linear Exclude 1/X Nona 56 Enabled 2 1 30.00 200.00 5.00 90.00 Disabled 30.00 ` 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled .pro\MethDB\110S99m.mdb Method Report Method file: Lest modified: Compound: Printed: r:\amelia backup sep99\amelie-] Mon Nov OS 01:20:27 1999C 3: Surr (Ch3) Hon Nov OS 0t:St:38 199 Compound Name: Internal Ref.: Quantify Trace: Cone, of Standards: User RF Value: User Peak Factor: Integrate Window Factor: Chromatogram mass window: Peak Location Retention Time (mins): Relative Retention Time: RT Reference: Time Window (mins): Peak Selection: Response Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Concentration Units: Noise Peak-to-peak amplitude: Smooth Smoothing: Window size (scansI: Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: Peak Seoaration Draw vertical threshold: Detect shoulders: Shoulder threshold: Resoonse Threshold Relative height: Absolute height: Relative area: Absolute area: Surr (Ch3) (None] TIC Fixed 1.000000, Disabled 1.000000 2.000 1.00000a 7.023, enabled 0.000, Disabled INone] 0.310 Nearest External Areas Linear Exclude 1/X None SO Enabled 2 l 30.00 200.00 S.00 90.00 Disabled 30.00 ' 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled .pro\MethDB\ 110599a .edb Method Report N.tnod lilt: Lsc modified: Compound: Printed: r : \ u i h . tuckup , . p \ . U-r.t..pro\M.thOBUI0599.-mat, Hon Nov 00 00:20:27 1999C 4: PFOSA (Ch4) Hon Nov 00 00:56:28 1999 Compound Name: Internal Rtf.: Quantify Tract: Cone, of Standards: Ustr RF Value: User Peek Factor: Integrate Window Factor: Chromatogram tail window: Ptak Location Rattntion Tint fains): Rtlative Rattntion Time: RT Rtftrtnct: Tint Window (ains): Ptak Stltction: Resoonse Rtsponst Type: Response: Calibration Curvts Polynomial Typt: Point of Origin: Fie Weighting: Axis Transformation: Concsntration Units: Noist Paak-to-peak amplitude: Smooth Smoothing: Window sizt (scans): Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: Peak Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: Resoonse Threshold Relative height: Absolute height: Relative area: Absolute area: PFOSA (Ch4) (None] TIC Cone. C 1.000000 Disabled 1.000000 2.000 1.00000a 7.770, Enabled 0.000, Disabled (None] 0.216 Nearest External Areas Linear Exclude 1/X None 82 Enabled 2 1 30.00 200.00 S.00 90.00 Disabled 30.00 . 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled ' AMELIA 062498: FACT Equipment Log 99114 Quattro II, #6448E 5 *PAGE DATE: 11/05/99 ANALYST: tas STUDY NUMBER: TOX145 MATRIX: rat liver DESCRIPTION: Day 29 control and dose FACT Method: ETS-8-7.0 Injection volume: 10 uL Cycle time: 10 min. Electrode: Z-Spray Mobile Phase: (A12.0 mM NH4CH3CQ2 (B lMeOH TN-A- or stndrd number (A) 99085-11-6 IBI TN-A-2997 Prepared (date/by): (At 10/30/99 sah_______ (B 10/29/99 mee Expires: (A) 04/00______________ IB) 04/00 Store at room temp? 0 or N Other:__ Guard column: None______________ Part number: na________Lot number: na Analytical column: Keystone B c t a s i l _____________________________ __ Size: 2 x 50 mm________________ Type:_C18___________ Sphere size: 5 urn_____ Part number: 055-701-2__________ Lot number P9E11 Serial number:089815 S Analytical parameters: Drying gas (LThr): 300 ESI nebulizing gas (L/hr) 10 LC Flow rate: 300 uL/min. Back pressure: 62 bar Sheath gas (L/hr)_0 HPLC solvent gradient: 10min-10-95 Time (min.)____ 1 ) 0 . 0 0 ____________ 2) 1.00____________ 3) 5.50________ 4) 7.50_________ 5) 8.00________ %B 10.0 10.0 95.0 95.0 lOB. . Tuning Method Report Method: C:\MASSLYNX\AMELIA062498. PRO\ACQUDB\PFOSl-6KV Printed: Fri Nov 05 09:43:09 1999 Page 1 SOURCE ( ESF ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. Sat Rdbk 1.60 40 5 0.2 150 250 1.60 -40 -3 151 253 Pressures Analyser Vacuum Gas Cell Rdbk 1.2e-4 4.8e-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set Rdbk 15.0 15.0 2.0 0.0 4 650 11 Set Rd] 14.0 14.0 10 2.0 0.0 40 0 650 12 10 10 canning Matnod Rapare Mathod i C :\MRSSLYI0C\AMEIJA0C298. F*0\ACOUM\1QKZII-Pr0#- PORA- XS-PTOSA U s e Modified: Mon Oct 11 07:22:17 1299 Printed: fri Nov OS 09:20:14 1999 Solvent Delay ( a i m ) : 0.00 Function : 1 MRM of 1 Haas Pair ( SSP- ) Inter Channel Cela/ 1i Secs > : Spen : Daltons . : Start Tiae ; M m s : End T:ae ( Mins : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) Coll Energy (eV) 1 413.30 169.00 0.30 30 Cone < V 15 Function : 2 MRM of 1 Maaa Pair < ESP- ) Inter Channel lei. Spar la.tir.i : Start rise M m s End 7.me t M m s : Repeats : Channel Parent 1 499.30 Sacs ) : Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) Coll Energy (eV) 99.00 0.30 45 Cone ( V 60 Ponction : 3 KRM of 1 Mai Pair ( IIP* ) Inter Channel De.a/ ( Secs ) : Span Daltons : Start Tiae M m s : End T:ae M m s Repeat : Chsrr.s. P-men*. Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) Coll Energy <eV) Cne ( V ) 1 l" . 1 80.00 0.30 40 90 Function : 4 MRM of 1 Mass Pair ( ESP- ) Inter Channel Del/ : Secs > : Span : Daltons ; Start Txae 1 Mins : End Time ( Mins 1 : Repeats : Channel parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) Coll Energy (eV) Cone ( V ) 43;. 78.00 0.40 45 60 Page i Method Report Method File: Last Modified Printed: C:\MASSLYNX\AMELIA0fi2498.PRO\ACQUDB\10min-10-95 Friday, November 05, 1999 06i22:24 Friday, November 05, 1999 09>26i28 Page HP1100 LC Pump Initial Conditions Solvents A% B% C% D% Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 90.0 10.0 0.0 0.0 0.300 10.0 0 400 30.0 30.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 5 entries which are ime 0.00 1.00 5.50 7.50 8.00 A% 90.0 90.0 5.0 5.0 90.0 B% 10.0 10.0 95.0 95.0 10.0 C% 0.0 0.0 0.0 0.0 0.0 D% 0.0 0.0 0.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 Pressure 400 400 400 400 40C ' HP1100 LC Pump External Event Timetable The Timetable contains 3 entries which are : Time Initial 0.00 0.10 Column Switch Contactl Off Off Off On Off Off Contact2 Off On Off Contact3 Off Off Off Contact4 Off On Off HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (jil/min) Draw Position (mm) Stop Time (mins) Injection Volume(/il) Vial Number 200.0 200 0.00 9.00 10-0 32 Masslynx - Sample Ust Sample List: C:\MASSLYNX\amelia062498.PRO\SampleDB\110599a.SPL Pnnted: Fri Nov 05 09:25:34 1999 Page Positior File Name File Text MS File 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 110599001 110599002 110599003 110599004 110599005 110599006 110599007 110599008 110599009 110599010 110599011 110599012 110599013 110599014 110599015 110599016 110599017 110599018 110599019 110599020 MeOH Blank MeOH Blank MeOH Blank TOX145-RBL11049-WBIk-1, RWW- Box 99-211 TOX145-RBL11049-RBL Blk-1, RWW- Box 99-211 TOX145-RBL11049-6ppt>-1. RWW- Box 99-211 TOX145-RBL11049-12ppb-1, RWW- Box 99-211 TOX145-RBL11049-30ppb-1, RWW- Box 99-211 TOX145-RBL11049-60ppb-1, RWW- Box 99-211 TOX145-RBL11049-120ppb-1, RWW- Box 99-211 TOX145-RBL11049-300ppb-1. RWW- Box 99-211 TOX145-RBL11049-600ppb-1, RWW- Box 99-211 TOX145-RBL11049-900ppb-1, RWW- Box 99-211 TOX145-RBL11049-1200ppb-1, RWW- Box 99-211 MeOH Blank TOX145-RBL, 9R03240-300ppb-MS, 11/4/99- Box 99-211 TOX145-RBL, 9R03240-300ppt>-MSD. 11/4/99 Box 99-211 TOX145-RBL, 9R03240/M/Day29/Control, 11/4/99 TOX145-RBL, 9R03241/M/Day29/Control, 11/4/99 TOX145-RBL, 9R03242/M/Day29/Control, 11/4/99 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 1MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 21 110599021 TOX145-RBL11049-300ppb-CC1-1, RWW- Box 99211 22 110599022 MeOH Blank 23 110599023 TOX145-RBL, 9R03243/M/Day29/Control, 11/4/99 24 110599024 TOX145-RBL, 9R03244/M/Day29/Control, 11/4/99 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOS A 10MIN-PFOS-POAA-IS-PFOSA 25 110599025 TOX145-RBL, 9R03255/M/Day29/5mg/kg, 11/4/99 10MIN-PFOS-POAA-IS-PFOSA 26 110599026 TOX145-RBL, 9R03256/M/Day29/5mg/kg, 11/4/99 27 110599027 TOX145-RBL, 9R03257/M/Day29/5mg/kg, 11/4/99 10MIN-PFOS-POAA-IS-PFOSA 10MIN-PFOS-POAA-IS-PFOSA 28 110599028 TOX145-RBL11049-300ppb-CC1 -2, RWW- Box 99211 10MIN-PFOS-POAA-IS-PFOSA 29 110599029 MeOH Blank 10MIN-PFOS-POAA-IS-PFOSA 30 110599030 TOX145-RBL, 9R03258/M/Day29/5mg/kg, 11/4/99 10MIN-PFOS-POAA-IS-PFOSA 31 110599031 TOX145-RBL, 9R03259/M/Day29/5mg/kg, 11/4/99 10MIN-PFOS-POAA-IS-PFOSA 32 1105S9032 TOX145-RBL11049-300ppb-CC1-1. RWW- Box 99211 10MIN-PFOS-POAA-IS-PFOSA 33 110599033 MeOH Blank 10MIN-PFOS-POAA-IS-PFOSA 34 110599034 TOX145-RBL11049-WBIk-1, RWW- Box 99211 10MIN-PFOS-POAA-IS-PFOSA 35 110599035 TOX145-RBL11049-RBL Blk-1, RWW- Box 99211 10MIN-PFOS-POAA-IS-PFOSA 36 110599036 TOX145-RBL11049-6ppb-1, RWW- Box 99211 10MIN-PFOS-POAA-IS-PFOSA 37 110599037 TOX145-RBL11049-12ppb-1, RWW- Box 99211 10MIN-PFOS-POAA-IS-PFOSA 38 110599038 TOX145-RBL11049-30ppb-1, RWW-Box 99211 10MIN-PFOS-POAA-IS-PFOSA 39 110599039 TOX145-RBL11049-60ppb-1. RWW- Box 99211 10MIN-PFOS-POAA-IS-PFOSA 40 110599040 TOX145-RBL11049-120ppb-1. RWW- Box 99-211 10MIN-PFOS-POAA-IS-PFOSA 41 110599041 TOX145-RBL11049-300ppb-1, RWW- Box 99211 10MIN-PFOS-POAA-IS-PFOSA 42 110599042 TOX145-RBL11049-600ppb-1, RWW- Box 99211 10MIN-PFOS-POAA-IS-PFOSA 43 110599043 TOX145-RBL11049-900ppb-1, RWW- Box 99-211 10MIN-PFOS-POAA-IS-PFOSA 44 110599044 TOX145-RBL11049-1200ppb-1, RWW- Box 99211 10MIN-PFOS-POAA-IS-PFOSA M asslynx - Sam ple List Sample List: C:\MASSLYNX\amelia062498.PRO\SampleDB\110599a.SPL Printed: Fri Nov 05 09:25:34 1999 Page 2 Page Position: (2, 1) Inlet File Bottle Inject Volume Sample Type Cone A Cone B Cone C Cone D Cone E Cone F 1 10min-10-95 91 2 10min-10-95 91 3 10min-10-95 91 4 10min-10-95 1 5 10min-10-95 2 6 10min-1Q-95 3 7 10mm-10-95 4 8 10mm-10-95 5 9 10min-10-95 6 10 10rrun-10-95 7 11 10min-10-95 8 12 10min-10-95 9 13 10min-10-95 10 14 10min-10-95 11 15 10min-10-95 92 16 10min-10-95 12 17 10min-10-95 13 18 10min-10-95 14 19 10min-10-95 15 20 10min-10-95 16 21 10min-10-95 24 22 10mm-10-95 92 23 10min-10-95 17 24 10min-10-95 18 25 10min-10-95 19 26 10min-10-95 20 27 10min-10-95 21 28 10min-1Q-95 25 29 10min-10-95 93 30 10mm-10-95 22 31 10mm-10-95 23 32 10mm-10-95 24 33 10min-10-95 93 34 10min-10-95 1 35 10min-10-95 2 36 10min-10-95 3 37 10min-10-95 4 38 10rnin-10-95 5 39 10min-10-95 6 40 10min-10-95 7 41 10min-10-95 8 42 10min-10-95 9 43 10mm-10-95 10 44 10min-10-95 11 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- FACT: DATA REVIEW SUMMARY FORM Dale: Data Analyst FACT Study 7 a s- Matrix/Timepoints: ~f)*j 2 9 duSt^ /ft/k im - f x / / / / f t Sam ple Lid: tno?i/L . Set-up Analysis Date/Analyst Instrument OZ4/1 Analyte: TAA (fu m e Acceptable Linear Range LOO l23rx> l RA2: O-VOZZL Matrix Blank Jess -/Luc*z Calibration Checks: 6f- MS/MSD: Dr.lfi. m o i n & s l ' /Pol A i r ^ A . Data Status: n . A j L nr. n h s h l Analvte: "PfS r. - P Acceptable Linear Range: /Z-53? i ------> n z t p p k ___ LOO: / i & p v L II R** fi. v w r r Calibration Checks: OK __ Extracted Blank fu ss 4L**.OQ Matrix Blank v& iJc'//** OQ - / 7 a MS/MSD: A)}" (in n U tri. lA tl'W + W - xarM1ilu Enk/U _ l -- ni irl Analyte: f fo S A C JZn*.c 3*) Acceptable Linear Range. t>-/3 w LOQ:. 1 RA2: 0 . 9 3 K /z z p L Wi Extracted Blank /e s s 4L . o q Matrix Blank frss y&M. CoQ Calibration Cheeks fk- MS/MSD: D aU U.ttA . P w A rom__ p n Q ^ il/ Data Sams: Dr> H I k M L C 111 Data Review Sipt-OfT Analyst Review / / Name/ Date: A S Technical Review . I, Name/Date: f E G J lh M __LiH ^Ipv-I$-^ Quality Assurance Review Name /Date: Data Entry: IA^ 11 J i l i j ________ Comments / Justifications:__________________ ________ Low / v J J M /u h : ( 2 o . Z > v d L. / ) iZf.re ? X ---- L jL is 4 L * ~JLl wf-fg_cilH. hlm -L----- &*Ji Pert w u j f j -from?-.------- 4 h Cosy* / J>Sj<U-a-li<i_ ------- K ina' 4 U Ma*j b u * l**n---------------- S/M ifiro-n-IL a //r k J A b & c / r o u m / firL J 4 J n/uiL-k - ^ 5" " t---- ) / L o u J C u u P t>d n J ~ . L . / p j > L . ----------- f d u c l a < / / M s n d J u J ij* . -/ ^ o /" CCtrsCu requinunA J - /U -------------- ttJ L J Jan. 4 L CU/ttee. vere eilaJualecI Oven- a f / w v h i m * .? p ro j> rte J c -- -fL J J a __ C ifm m iv d ' to ( T ) : P o A fi \M (t (U tf- 0 ~---------j A A J ~ a u /t!? H p /- ^ '\ y jM e k b d ' u L -- k j * t V ' l ^ __________ 3*s j . //Z' FACT: DATA REVIEW SUMMARY FORM D ate Data Analyst: "Iks FACT Study: T o tr .------------------------------------------------------ -- Matnx/Timepoints: . k y & iL t U in Sam ple L ilt Ht o f f -------------- ---- ------------------------------------------- Set-up Analysis Date/Analyst Data Review Sign-OfT Analyst Review n rName / Date:__ "A ik TeebakalReview r, Name/Date: Ra&r -U pay. |, -- liji/9 Q uality Assurance Review Name / D ale:___________ _________________________________ Data Entry: 1AL. ulirhl 5- ^ 2vf-2~ ! i 6 s i i S 8 "pWYl -fOM 'O pJp '3^1'OUO 3 S asSaSrsc. gggggsssb S SSB SSSS s g 4 5 w SskSSSsss S g SsssBscoooo S SSSSgggg 3 ,,SiSSgg f BsSHSsSC., gggggggg 444444g4444 SSassSSSSSS slsS S S a S S s ss " h % . 00 gsssssagggg -CSKCSu. ! MNK *E-q44oorT' 6 O m n - 5 T X a i' CC0S60IIT CC MHOV0>J(lUI*WKIH<A(iv|fiUIkWMHO<4>lUI^UMHa 3 I m i ooooooooooooooooooooooooooooooooB oooooooooooooooooooooooooooooooo UWWMMMMMMMNMMHHHHHMHHHHOOOOOOOOO i ?SI 1 t* * ** Krt &r aaaaaaaaaaiaaaaaasaaaaaaaaaaaifir EseKSSssPBgsecHeslEssppesgEcBllll UIUUVIWW^VMVUIWUIVMuiRMWIVU(giWW<tfiWiUIVI|iaM i B6S5S3SSSB|B333|BBBS55353SS| E E E E E E E E E E ^ E r r r r r f r E E C E P E E E P E E * * 8''' h m m m m m m h h m m -' i< 0 0 0 00000* 0* 0 * * V o o*o.o* o o o o.oo o B OOOOO rt 1 I I I I I I I 1 I UWWUW t t I I I I t I I I I O O O W O O W H M OUMDUIWW M O O O M O O K I f l & i *" r w ! s s f i l i l i f f i f i H i l s ? N N NJWT"w w w M1 . T ln lgVg n| o| ST Ni MT MTWi >m n n - M1 . "i' Il C ir ?ir w n* caia 1111 od ago 00000 00000 mi ih ! rp in i K ? `V i i \\ HHHMH p H HP M s 0(ftWUMUIIAM rt rt n r* n n n n II i UH oaooswH iUH JMHOHUH IHPvIUPOWO s l m m m m m m m u m m m m m m m u m m m m m m mm wuu>gioguHHPaHuiookuiawioi 3 tZZ'L OO'BZZX pxwpa**S C9CCT * MUMHM U>UiUJHI W >MMH<JOP u g gggggggg%gi8888888i ggggggigf lgggggj UWH UUUMMM HWH ! I3 r! ii! ISIS till !SiS ..? i UH H M M ISiSS IQ O O M N N r * vt n h 10r f'*ooo0Ooinoeoirtr4nHO<< 5i i i i i 5i 55i 55i i i 5i i S 5i i a 5i 55S i i i i ?**- > * r* #r r*o tn*m faH nr B o r o o > n M n H N M n M M a 'NaoerH>*iiftonfir MnmnnnrtHriHNHHHc trr*f*r*r*rr*f*t*r*rr OHr*Hor 4 H HnOnHira a rr ' f h i a OH w rrttor rto hn cr Hn it r 3-- <5" \f\ o 3 c<y iiHiJiU otr r otv c o 1 . 1S i l l * fi . 'NNiiri Qi D OI O D VOBDS 1M M S 2 9 m i rX S, > - - H i 'I N N N N H >, S >. >.f aam ^ ,i|lili i* IXXlj 5 911 Bn o o n o o o js sa K O O >* I >0000000 oooooooooc HHHHHHHHHH ' H HHHHHHHHHHH ?lll??22222325S9kfcfckt23S52S2S32S2S i Irt *> t/tu t M r r r i A rniAr MiAn * * * g g g g g g g f > g e l g g g g g f Jggggggggggg 3""3 c a 3. TS Co J Jo *3 OOOOOOOOOHHrtHHrtHHioooooooooooooooooc 3O O O OO C tAOrtrtn IO O O OOOO OOOO OOOO OOOOC 30000000000 a) a o * ** n r* n r rat 1 1 m , day ]} tea* dilatlem* axt. 11/4 / M I *7 *t 1 ' 1 1 * * * f o * h m m M i r>o**oAOooeoehoaooHoeo 0000*4000HOOOOOOQOOOOOHr4HHOOHMO aaaaaaaaaaasaaaaaasaaaaaaaaaaa l onaHhtevBitin o4 rt >iooaoNf OO Ht rh<Ho^th' OOn0*niA0<4<1hMANaHHOnO4a0440 ,1 O Q ' i ! ? e * * ,,g'a o * ri^ o o a o o a i ' a a H H M H O O O H O O O O O rtO H H H M H H O O rtO O O O O O r* r r-r* r r- r r- i- .f r r r* r r- r* f r ooooooooa oooooooeo -21 ~vH hUkiiuhl ' lU ll; m lini o 3 i s 0> 9t 2i s* H mh n 59 r r4 ! 3o * 3 r r> o OQaQO SSSSSi h in ~ J8 "3 I1*!11*11. SRRSS ^ n-i^i`llii i l !i S* 5m O O N O D O fl I >* S O O O O O O O- O- O- ma iSlV! MI M mn r r r> r r I O O a O O O' *< * * * * * .7 . ^ 7 7 7 7 4 fiiitiltil S.2 r ,, ,, . e o e s n a e o o r o o o n MrinwHn4iH ............... .. ooooooooooo J- ""3 c. e5 Jli ?ifi IH = 3 I*; fisl sssssssassssssas&Ealsssasssasss a B aminiAininiAiAifliiAiAaiflMiAinMAflMMMtfiiAviiAininiAiA "o ! fg m ee em g m e eP m P e g P g m tfl- U- <4 i s iO i> a M V3; . Qu*atlfy i hm t M ? r! u d u a OOOOOOOOOHrfrlrtiJHHHHHMNMNNMflHMM'inMrt ooooooooooooooooooooooooooooooooo IIo o o oooooooooooqoooooooqooooooo o 8 S i * 1 t 8 i 0301991 Qu*ntlt*t*4 ad printed by ! 11/11/99 Pa0 2 totip 0201i Quneltaeo4 tad prlatod toy l" 11/11/* Pmgm 1 oup Q301t>: Qu*atlt*td ad printed toy i" * 11/11/99 9*0 * toyloup 020199 : Quantitt an prit i * 11/11/99 Method Report Method file: Lest aodiied: Coevound: Printed: C \HA5SliY7nC\,oup020173 .pro\HtiDU110** " > Thu H v 11 07:01:12 U 9 X: PORA (Fune 1) ThU OV 11 07:3*:* 9 CoMpound Mese: Internal Ref.: Quantify Trace: Cone, of Standard*; User tr Value: User Peak Factor: Integrate Window Factor: Chromatogram nasa window: PORA (Fune 1) nc(Monel Cone. A 1 .000000, 1.000000 2.000 l.OOOQDa Oieebled Retention Tin* (nina): Relative Retention Tin RT Reference: Tin* Window Inina): Peak Selection: 7.0S7. 0.000. (Monel 0 .2 * 0 Enabled Disabled Mearost Response Type: Response : External Areas Polynomial Type: Point of Origin: Fit weighting: Axis Transformation: Linear esclude 1/X Mone Units: Peak-co-peak amplitude: smoothing: Window sise (seana) Number of smooths: Smoothing method: join valley threshold: Redue* peak tailing: Rais* baseline maxisum: 12 Enabled 2 1 30.00 200.00 5.00 Draw vertical threshold: Detect shoulders: Shoulder threshold: Relative height: Absolute height: Relative are*: Absolute area: 00.00 Disabled 30.00 1.S0, Disabled 0.00. Disabled 2.00, Disabled 0.00, Disabled rf*[lT ' 9 1 Method Report Method Cile: Lest Modified: COMpound: Printed: C i\ll*S S L Y ia \*o u p O JO m .p ro M < O lD *\1 1 1 0 - < > na Mov 11 07:08:22 lt99 2: pros (Pune 2) Thu Mov 11 07:34:44 1*' ________ C e ^ o u o d Mene: Intemel Ref.: Quantify Tree: Cone, of Standards User RT Value: User Peak factor: Integrate Window factor: Chromatogram Mass wiodow: pros (Pune 2) (Mone] TIC Cone. B 1.000000. Diaatolod 1.000000 2.000 l.OOOODa Retention Tine (nine): Relative Retention Tine: RT Reference: Tine Window (mins) : Peak Selection: 7.284, Bnabled 0.000. Disabled (Menai 0.279 Nearest Response Type: Response : External Areas Polynoaial Type: Point of Origin: Pit weighting: Axis Transformation: Linear Exclude 1/X Mone Units: Peak-to-peak amplitude: Sneothing: Window size (scans) Number of ooths: Smoothing method: Join valley threshold: Reduce peak tailing: Raise baseline nav i Draw vertical threshold: Detect shoulders: Shoulder threshold: Relative height: Absolute height: Relative area: Absolute area: 98 Bnabled 2 1 30.00 200.00 S.00 90.00 Disabled 30.00 1.50, Disabled 0.00. Disabled 2.00, Disabled 0.00. Disabled 9*0 2 Method Report Method 1: Lest modified: Compound: Printed: C: M O S S tn iIV .~ P 0 2 0 1 i.p ro \H .t M B M 1109... Thu Nov 11 0 7 :0 1 :2 2 1*** 4: Surr (Func 4) Thu Nov 11 07:34:44 1953 Compound Marne: internal Mt . : Quantify Trace: Cone, of Standard: User W Value: User Seek Factor: Integrate Window Faetor: Chromatogram ass window Surr (Func 4) (Monel TIC Fixed 1.000000. Disabled 1.000000 2 .0 0 0 l.OOOODa Retention Time (nine): Relative Retention Time: RT Reference: Tine Window (mine): peak Selection: 7.1(1, Enabled 0 ,000. Disabled (Monel 0.278 Nearest Polynomial Type: Point of Origin: Pit Weighting: Axis Transformation: Units: peak-to-peak solitude: Smoothing: Window si*e (scans): Mrnber of smooths; Smoothing method: join valley threshold: Reduce peak tailing: Raise baseline maxisaa: Draw vertical threshold: Detact ahouldars; Shoulder threshold: Relative height: Abaolute height: Relative area: Absolute area: Linear Exclude 1/X Mone 92 enabled 2 1 30.00 200.00 S.00 90.00 Disabled 30.00 - 1.50. Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled Quattro II, #6414E "/b in SOUP 020199: FACT Equipment Log 99092 PAGE 1/1 DATE: 11-10-99 ANALYSTnas MATRIX: rat liver DESCRIPTION- dilutions-day29 STUDY NUMBERilQXHl FACT Method: FTS-8-7.0 Injection volume: 10 uL------ Cycle time: 10 min. Electrode:.Z-Spray--------- Mobile Phase: ( a-)? n mM NH4CH3CQ2 (B)MeQH------- TN-A- or stndrd number (A) 00085-11-21----------- (B)JN-A-3??i Prepared (date/by): f 11/ft/QOah (B) 11//99 sah-- Expires: l'A 04/00 ---------------- (B)_2Q1Q------- Store at room temp? @ or N Other:--------- ----------------------- Guard column: None Part number:ja_____ Lot number:jra Analytical column:jleystgneBetasiL Type: C l8_______ Size:_2jL50jEOE____ _______ _-- Part numher 055-701-2--------- --- Lot numher: P9E11 Sphere size: 5 um----------- Serial number:059Jj5Q4Z Analytical parameters: Drying gas (L/hr):_25Q___ ESI nebulizing gas (L/hr)_0----- Sheath gas (L/hr)JL LC How rate:JQ0uUmiIL Back pressure: $5 bill-- HPLC solvent gradient: 10min-10-95 Time (min.l n o.oo - 2) _L2Q------ 3) .L5Q___ 4) i 5 0 ____ 518.00 _ %B 10.0 10.0 j ia 95.0 10.0 Tuning Method Report Method: c :\MASSLTOX\SOOP020199.PRONACQUDB\PFOS3 Printed: Wed Nov 10 10:49:41 1999 Page 1 SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. get Rdbk 1.60 40 5 0.2 150 250 1.61 -60 150 250 Pressures Analyser Vacuum Gas Cell Rdbk 4.le-3 MSI LM Resolution HM Resolution ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set Rdbk 14.0 14.0 0.9 0.0 4 650 3 Set Rdbk 14.0 14.0 10 2.0 0.0 40 0 650 37 38 40 Method Report Itathod Fila: Last Modified: prlncad. 8F1100 1C Pump Initial conditlona Solvents A% B% C% D% Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) HV1100 LC Pump gradient Timetable C:\MAflSLYSxV800P020199.VRO\ACOmJB\10mln-10-95 ,,dnesday, Movaaier 10, 1999 10.3*07 1 Wednesday, November 10, 1999 10:49:20 _______ ____________ 90.0 10.0 0.0 0.0 0.300 10.0 0 400 30.0 30.0 Time 0.00 1.00 5.50 7.50 8.00 A% 90.0 90.0 5.0 5.0 90.0 B% 10.0 10.0 95.0 95.0 10.0 C% u .u nn nu .uft nu .fVt 0.0 HF1100 LC Pump External Event Timetable The Timetable contains 3 entries which are : Time Initial 0.00 0.10 Column Switch Contactl Off Off Off On Off o f f Contact2 off On Off HP1100 Autoaaapler Initial Conditions Draw Speed Eject Speed (ul/min) Draw Position (mm) Stop Time (mins) Injection Volume (ill) Vial Number 200.0 200 0.00 9.00 10.0 91 D% Flow 0.0 0.300 0.0 0.300 0.0 0.300 0.0 0.300 0.0 0.300 Contact3 Off Off Off Contact4 Off On off Pressure 400 400 400 400 400 Masslynx - Sample List < Sample Ust: C:\MASSLYNX\soup020199.pro\SampleDB\111099a.SPL Printed: Wed Nov 10 10:48:56 1999 Page Position: (1,1) File Name File Text MS File 10MIN-PFOS-POAA-PFOSA-IS 1 111099001 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 2 111099002 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 3 4 111099003 MeOH Blank 111099004 TOX145-RBL11049-WBIk-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 5 111099005 TOX145-RBL11049-RBLBIk-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 6 111099006 TOX145-RBL11049-6PP-2, RWW 7 8 111099007 TOX145-RBL11049-12ppb-2, RWW 111099008 TOX145-RBL11049-30ppb-2, RWW 9 10 11 111099009 TOX145-RBL11049-60ppb-2, RWW 111099010 TOX145-RBL11049-120ppb-2, RWW 111099011 TOX145-RBL11049-300ppb-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 12 13 111099012 TOX145-RBL11049-600ppb-2, RWW 111099013 TOX145-RBL11049-900ppb-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 14 111099014 TOX145-RBL11049-1200ppb-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 15 16 17 18 19 20 21 111099015 111099016 111099017 111099018 111099019 111099020 111099021 MeOH Blank TOX145-RTL, 9R03255/M/Day29/5mg/kg-D100, 11/4/99 TOX145-RTL, 9R03256/M/Day29/5mg/kg-D100, 11/4/99 TOX145-RTL, 9R03257/M/Day29/5mg/kg-D100, 11/4/99 TOX145-RTU 9R03258/M/Day29/5mg/kg-D100, 11/4/99 TOX145-RTL, 9R03259/M/Day29/5mg/kg-D100, 11/4/99 TOX145-RBL11049-300ppb-CC1 -2, RWW 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 1OMIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 22 111099022 MeOH Blank 23 111099023 TOX145-RBL11049-WBIk-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 24 111099024 TOX145-RBL11049-RBLBIk-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 25 26 111099025 TOX145-RBL11049-6ppb-2, RWW 111099026 TOX145-RBL11049-12ppb-2, RWW 27 111099027 TOX145-RBL11049-30ppb-2, RWW 28 111099028 TOX145-RBL11049-60ppb-2, RWW 29 111099029 TOX145-RBL11049*120ppb-2, RWW 30 111099030 TOX145-RBL11049-300ppb-2, RWW 31 111099031 TOX145-RBL11049-600ppb-2, RWW 32 111099032 TOX145-RBL11049-900ppb-2, RWW 33 111099033 TOX145-RBL11049-1200ppb-2, RWW 34 111099034 TOX145-RBL11049-900ppb-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-1S 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS o ooco i i ! 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