Document zbx9Vxjv20NJyDBxrmRY6m8va

3M 3M Environmental Technology and Services PO Box 33331 St. Paul, MN 55133-3331 612 778 6442 $-6H$ - 8C0~ 3 73 -0051 Laboratory Report Report of Data for Exploratory 28-Day Oral Toxicity Study in Rats: Telomer Alcohol, Telomer Acrylate, , PFHS, PFOS Laboratory Report No. FACT-TOX-120.3 Requester Project No. NOTOX #242933 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 CmCll i *---j ---DvjnmOT -'-J C'23Crn3 ID r r> rc c u > - <- - u f -i*;*'- U-^ . C - L. Cv CS> rD v^c 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 Marv Case and Paul Lieder 3M Company Toxicology Services 220-2E-02 St. Paul, MN Report issued 6/11/99 & E P A -O T S 000811788X O G oaii7flax 000448 3M ENVIRONMENTAL LABORATORY REPORTNO. FACT-TOX-120 This study was designed to preliminarily assess the toxicity o fvarious test articles to die female Sprague Dawley ra t Test animals were dosed by oral gavage at the following levels: Group 2: Telomer Alcohol Group 3: Telomer Acrylate Group 4: Group 5: PFHS G ro u p 6 :F F O S 30 mg/kg/day 30 mg/kg/day 30 mg/kg/day 10 mg/kg/day 3 mg/kg/day W ithin each group, 8 animals were given test material each day for 28 days, and then sacrificed. Three animals were allowed to "reco v er (no test material) for 14 days before sacrifice; three animals were allowed to recover for 28 days before sacrifice. liv e r samples collected from the sacrificed animals were sent to the Environmental Lab and analyzed quantitatively for perflnnmoctane sulfonate (PFQS) and other perfluorinated, sulfonate-based or carboxylic-- a d d based metabolites. (A full list o f acronyms and formulas is attached in Attachment B). Tissue samples were homogenized (liver) and extracted using an ion-pairing extraction procedure. The .extracts were quantitatively analyzed using high-pressure liquid chromatograpby/electrospray tandem mass spectrometry (HLPC/ESMSMS), and evaluated versus an extracted curve. Analytical details are available in the study hinder maintained by FACT. The presence or absence ofknown fluorochemical contaminants and metabolites is determined by inspection Six perfluorinated carboxylic adds were identified in the liver sample extracts derived from both group 2 and group 3 animals (see Attachment D). Forgroup2 and group 3, livers from male and female animals in both groups ofrecovery animals showed a decrease in the concentration o f POAA. The concentration of two other carboxylic ad d based flnnnyhem iralg measured qnantitatively (M513, M613) did not show as significant a decrease over the recovery period The concentrations ofthree other carboxylic add-based compounds could not be determined, as standard material is not available. Other perfluorinated or partiaHy-fluorinated metabolites may be present in the rat liver samples analyzed, but these compounds cannot be confirmed without standard material Relative to PFOS levels in the corresponding group 6 animals, (group 4) and PFHS (group 5) levels determined in liver samples showed a dramatic decrease in the day 14 and day 28 recovery groups. W ithin each group, samples showed a relatively large standard deviation which may indicate variability in dosing or in metabolism o f the test compound W ith the exception o fPFOS-dosed animals (group 6), there were dramatic differences in target analyte levels in livers o f male and female animals. For example, livers from 14 day recovery group 5 females animals were determined to contain two and a half enters o f magnitude less PFHS than the corresponding male animals Although rigorous quality control measures and 3MEnvironmental Laboratory Standard Operating Procedures were followed, the acquisition o fthis data was not necessarily collected according to applicable Good Laboratory Practices. This data is not suitable for distribution to any government agency in defense of product suitability or safety. Data presented here is tire highest quality data available at this time. This summary should notbe considered to be a complete inventory of all metabolites associated with the test m aterial Analyte measurements were made only on those compounds deemed by FACT as likely to be . present Certain other compounds have been identified but cannot be quantitated as standard material is not available. 000449 3M ENVIRONMENTAL LABORATORY REPORTNO. FACT-TOX-120 Liver samples arrived frozen at the Environmental Lab on 2/3/99. A chain-of-custody was not submitted w ith the samples, but was initiated upon receiptby die Environmental Lab. There is no holding time criteria associated with these samples for LC/ESMSMS analysis. Analytical methods FACT-M-1.0, Extraction o f Potassium PerQuooctanesulfonate or Other Anionic Photochem ical Surfactants from Liver for Analysis Using HPLC/ESMS FACTVM-2.0, Analysis ofFluorochemicals in Liver Extract Using HFLC-Electrospray/Mass Spectrometry Sam ple p reparation - aqueous sam ples, HPLC/ESM SM S: ion-pairing extraction *. Analyte is extracted from a sample matrix with ion pairing reagent [tetrabulyl ammonium hydrogen sulfate (TBA)] in a pH-controlled environmenL The cationic reagent selectively targets anionic fluorochemicals. Once die anion-TBApair is formed, die analyte is transferred into a non-polar organic solvent (methyl-terfbutyl ether),' dried, and reconstituted in methanol for MS analysis. HPLC/ESM S and HPLC/ESM SM S: fo r detailed qualitative w ork . In HPLC, an aliquot of extract is injected and passed through a reverse phase liquid chromatographic column. Based on the affinity o f the analyte for the stationary phase in the column relative to the liquid mobile phase, the analyte is retained for a characteristic amount of time. For example, in a standard solution PFOS may elute at 5.0 minutes. Retention times between a standard EPOS solution and the analyte extracted from liver in this analysis were matched on the HPLC system to within 1%. ... . . Following HPLC separation, ESMSMS provides a rapid and accurate means for analyzing a wide range o f organic compounds, including fluorochemicals. Electrospray, an ionization technique used primarily for detection o fmolecular ions, is generally operated at relatively m ild temperatures. Molecules are ionized, and a primary inn, characteristic o f the analyte, is selected This ion is bombarded w ith high-energy gas; subsequent collisions create smaller secondary ionic fragments unique to the primary ion, which are detected. ,-x For example, for PFOS (CgFnSQO analysis, ion 499 is selected as the characteristic primary ion. This ion is fragmented into other ions such as 80 am u (corresponding to SOs"), an d 230 amu (CjFsSCV). Each o f these secondary fragments is detected and can be used to differentiate PFOS from other compounds that m ight have the same characteristic 499 am u primary ion, but different chemical compositions and secondary ion fragmentation patterns. 5.1 Calibration A mid-level, extracted matrix calibration check standard is analyzed every 5-10 samples to monitor instrumental d rift Calibration check standards are compliant if instrumental response is within +/- 30% o f the expected value. 0004S0 3MENVIRONMENTAL LABORATORY REPORTNO. FACT-TQX-120 Quantitation ofthe target analytes is based on linear regression analysis (weighted 1/x, if appropriate) o f two extracted matrix curves bracketing each group o f samples. Quantitation of each analyte is based in the response o f one or more specific daughter ions using the multiple response-monitoring mode o f the instrum ent 5.2 Blanks Two extraction blanks, utilizing water as surrogate matrix, are extracted with each batch of samples. Additionally, two samples ofblank matrix, used for the extracted calibration curves, are extracted along with each batch of samples and curves. Blanks are compliant if no target analyte is detected above the limit of detection for a specific analyte. In this study, all blanks were compliant 5.3 Surrogates Tetra-bydro perfluorooctane sulfonate is used as a surrogate in this analysis. Surrogate response is monitored to confirm gross instrumental failure, if necessary. 5.4 M atrix Spikes Duplicate matrix spike analyses utilizing all target analytes were prepared and analyzed for one control animal Except as noted in the results table, recoveries were within the acceptable range o f 70-130%. Recoveries outside this range may be re-evaluated. 5.5 Laboratory Control Samples Laboratory Control Samples are not a component o f this study. Six perfiuorinated carboxylic adds were identified in the liver sample extracts derived from both Group 2 and Group3 animals (see Attachment D). For group2 and group 3, livers from male and female animals in both groups ofrecovery animals showed a decrease in the concentration of POAA Ih e concentration of two other carboxylic a d d based fluorochemicals measured quantitatively (M 513, MS13) did not show as significant a decrease over the recovery period. The concentrations of three other carboxylic arid-based compounds could not be determined, as standard material is not available. Other perfiuorinated or partiaUy-fluorinated metabolites may be present in the rat liver samples analyzed, but these compounds cannotbe confirmed without standard material Relative to PFO Slevds in the corresponding group 6 animals, (group 4) and PFHS (group 5) levels determined in liver samples showed a dramatic decrease in the day 14 and day 28 recovery groups. W ithin each group, samples showed a relativdy large standard deviation which may indicate variability in dosing or in metabolism o fthe test compound W ith the exception ofPFOS-dosed animals (group 6), there were dramatic differences in target analyte levels in livers o f male and female animals. For example, livers from 14 day recovery groups females animals were determined to contain two and a halforders o f magnitude less PFHS than the corresponding male animals These results indicate that ingestion of each of the test materials leads to some accumulation o f metabolites in the liver. Relative rate ofdearance can be determined. 000451 3MENVIRONMENTAL LABORATORY REPORTNO. FACT-TOX-120 Samples and extracts willbe retained for future evaluation, if necessary. 9.1 A ttachm ent A : Table of Results o f Analysis o f Liver Samples 9.2 A ttachm ent B : Table of FACT acronyms and form ulas 9.3 A ttachm ent C : Graphical Results by Group and Gender 9.4 A ttachm ent D: Chromatographic results ofPFC A investigation in Group2 and Group 3 9.5 A ttachm ent E : Chain o f Custody 9.6 A ttachm ent F : Analytical D ata i 000452 3 M Environm ental Laboratory Fluorine A nalytical Chem istry Team fFACQ FACT-TOX-120, R at Livers 28-D ay O ral Tox Study b y D aily Gavage in Rats PFOS (C8F 17S 0 3') (Female) ..G1 ' G6 Dayl Day 14 Day28 0.086+/-0.046 0.102+/-0.020 0.329+/-0.060 377+/-31 240+/-25 191+/-15 j[M ale2__ Dayl Day 14 Day28 G1 0.133+/-0.030 0.255 +/- 0.122 0.099+/-0.007 G6 419+/-86 309+/-34 237+/-25 PFHS (C6F l3S O i ) (Female) G1 G5 Dayl <MDL 97.0+/-14.7 Day 14 <MDL 0.26+/-0.12 Day28 <MDL 0.03+/-0.01 (Male) G1 G5 Dayl Day 14 Day28 0.055 +/- 0.020 0.129+/-0.088 0.089+/-0.019 327+/-52 61.9+/-11.7 36.3+/-7.4 (Female) G1 G4 (Male) G1 G4 (7 Day 1 <MDL 0.37+/-0.38 Day 14 < MDL 0.02+/-0.00 Day28 <MDL <MDL Dayl <MDL 3.09+/-1.58 Day 14 Day28 <MDL <MDL 0.126+/-0.084 0.025 +/- 0.015 3M Confidential 000453 3 M Environm ental Laboratory Fluorine A nalytical Chem istry Team FACT FACT-TOX-120, R at Livers 28-D ay O rai Tox Study b y D aily Gavage in Rats POAA (C 7f 15c o 3 ) (Female) Gl G2 G3 (Male) Gl G2 G3 Dayl <MDL 0.164+/. 0.035 0.112+/-0.039 Day 14 <MDL 0.016+/-0.010 <MDL Day28 <MDL <MDL < MDL Day 1 <MDL 6.59+/-2.16 8.64+/-1.48 Day 14 <MDL 3.59+/-0.67 3.36+/-1.65 Day28 <MDL 1.76+/-0.23 1.26+/-0.44 MS13 (C9F 19C 0 2') (Female) Gl G2 G3 ___ (Male) Gl G2 G3 Dayl <MDL 1.69+/-0.18 1.20 +/-0.30 Dayl <MDL 1.91 +/- 0.88 1.78+/-0.31 Day 14 <MDL 1 .3 6 + /-0 .0 2 1.20+/-0.09 Day28 < MDL . 2.24+/-0.22 0 .8 1 2 + /-0 .1 8 8 Day 14 <MDL 1 .7 3 + /-0 .4 6 1.08 +/- 0.26 Day28 <MDL 1 .5 2 + /-0 .3 2 0.801 +/- 0.148 M613 (Cn F 23C O i) (Female) Gl G2 G3 . (Male) Gl G2 G3 Dayl <MDL 0.117+/-0.020 0.029+/-0.017 Day 14 <MDL 0.085+/-0.019 0.035 +/- Qj015 Day28 <MDL ' 0.101+/-0.012 0.036+/- 0.011 Dayl <MDL 0.087+/-0.015 0.0622 Day 14 <MDL 0.107+/-0.041 <MDL Day28 <MDL 0.106+/-0.017 < MDL ** C9, C l l and C13 perfluorinated carboxylic acids also detected in G2 and G3 animals 3M Confidential 000454 000455 FAC. :-no 2S-Day Oral Tox Stndy by Daily Gavaje la Rata MfroditokclM nA o(rca S aM a); MutoMnU! 6 Softwm/VcnioK DM TEraaoka/AatlyM: DM *fAaalyili/Aailya: DM TDM R eM M A adj; Sim ple Data TO X -!2C lExplorM (y2U )*yO nlTaxkityStsdybyD n!yG m geiiX T-7023,T-7Q24, T-7022, T-7032, T-4295 iM L iw IH om bc: FACTMI4St PACMK-2.0 R-Squred V ahe So^COOl, H u tte 041090A--fil 0C49I Siepe M d.yn3.l Y -h tan p t 2/22*9 RWW/SAH 02/23* 9, 03/01* 9, 03/ 11* 9, 05/23*9 ho j/m b b /d r b 02/2S*X 03/00*9, <0/12/99,05/26*9 ME8/DKB/KJH/H0J to A m tlw e iM faeA U M teau Sm AttacfctMett RATUVER Gmp Dm M eted B& M eted BUt M aris BUt M arijB ft QC-M O n* QC-M OfH Greep 1 ana(W qr OM I G m pl 0.0 a g i o te Rm m o vM 4 D m C risp OOafteM qr iM v a v l'ltD m CffM f> 30.0pAffidap Tdom a Akohel C rap l 3 0 .0 a fi|9 t)r Recovery 1 !4Dyv C rap l 30.0fA f/day Recovar 2-2$ Dey C raf] 30.0apg/dry Tckw rA nyiM GreopS Recovay I 14Deyt rap i N O opldqr Recovar 2 21 Poye Sim ple EstrsdedW k 1 H20Bik-l H20B&-2 X iU llU n rB ir R teciU verB lk-2 106F 106F 1IQF IIOF 97F 91F 99F 100F 101F 102F 103F 104F 105F 106F 107F 109F 110F II1F 114F 115F II6F 117F IIBF 119F 120F 12IF 122F 123F 129F 126F 127F I29F . 130F 131F 132F 133F 134F 135F 136F I37F 130F 139F 141F 142F 143F NA NA NA NA 0.9240 0.9240 0.9242 0.9242 0 2 I 0.4339 03106 0390* 0.6970 0.4313 0.4901 OII16 0.6936 0.9240 0.43S9 0.4110 0920 0.9429 03506 0.649S 16769 0.7235 0.6534 0.4162 03791 0.4295 0.0372 0.6291 03660 0.1074 09112 0.6006 0.4M1 0.3012 0.7303 0.5990 0.3011 0.6131 0.5369 03799 RIOM 0.6235 0.5600 0.6693 0.7953 0.7303 MS C ifeC ac. Fl <MDL <MDL <MDL <MDL 251 250 99 190 67.2 70.1 64.9 9007 Ni 653 62.0 119 106 00.6 344 379 263 4L3 33.7 37.1 364 OU 564 30.0 294 354 314 473 4U 513 524 343 3M . 514 413 494 453 35.7 46.1 17.9 194 43.9 42.4 413 403 T etti A m eut eTPVOS ufi <MDL <MDL <MDL . <MDL MK S4K 23% 3394 0190 00672 00701 00649 941 . 00765 00655 00630 0119 0106 00006 0344 0379 0263 00412 00937 O03TI 00366 00016 00569 00310 00295 00356 00354 00473 00452 00505 00520 o.aW i 00304 00516 00415 . 00496 / 00152 00357 00460 00179 04194 00439 00424 00413 00402 M ctM Dcicctm Liait (M Dt F fO S 23*fe,raA A -S *fcM 5U -2S m dS O ^rg,M S13*25*fe A vertit FFOS Fl <MDL <MDL 15% 2394 00063 130 0103 0329 00443 00394 00519 00429 00271 00413 Dm Eatocd/Anly*: DM VsifUd/Aaaiyvt: 02/2699,63/01/99,03/22*9,05/2699 LAC 06*0*9,06/09*9 EAD RSD M .D cv. <MDL <MDL 394 NK 53.4 >00461* 263 3.15 193 00196 113 00597 314 00171 173 000614 124 000667 154 000644 519 00146 170 000112 FOAA Cale. Cese, rafie <MDL <MDL <MDL <MDL 219 267 i k 17172 0.00 OOO OOO 000 OOO OOO OOO OOO OOO OOO 0.00 OOO OOO OOO 13 ns 163 160 105 196 223 139 243 433 17.4 0 0 0 4J 105 954 166 124 906 170 75.1 OOO 000 OOO OOO OOO OOO T etti A m ari efFOAA rt <MDL <MPL <MDL <MDL 7394 0994 75% 53% <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL 0135 0115 0163 0160 0105 0196 0223 0139 04245 000453 00174 <MDL <MDL <MDL 00665 0105 00950 0166 0124 00906 0170 00751 <MDL <MDL <MDL <MDL <MDL <MDL NX NoiR^orted N/A-Not Applicale m s- K )A A M513-C9P19COO- 16613* C lIF23CDO A verti FOAA Fk <MDL <MDL 01% 66% <MDL <MDL <MDL 0164 0015) <MDL 0112 <MDL <MDL RSD StODcv. <MDL MDL 20% 25% <MDL <MDL <MDL ILS 00354 6X4 00101 MDL 354 04390 MDL MDL Citc.Ceec>- Ft MDL MDL MDL <MDL 122 193 122 193 OOO OOO VALUS OOO OOO OOO . VALUS VALUS VALUS VALUS VALUS VALUS VALUS VALUS VaLUb VALUS VALUB VALUS VALUS VALUS VALUS VALUS VALUS VALUB VALUS VALUS VALUS VALUS avau VALUB VALUB VALUB VALUB VALUS VALUB VALUS VALUS VALUS VALUS VALUS VALUS VALUS T etti A eusat ef Fl <MDL <MDL <MDL <M0L 41% 65% 41% 65% <10 H* to n * NR <n* n * to n * NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR . NR NR NR NR NR NR NI NR NR NR Ml NR NR NR NR A vertit Fl <MDL <MDL 53% 53% NR NR NR NR NR NR NR NR NR A d. Dm <MDL <MDL 46% 46% NR NR NR NR NR NR NR NR NR FACT-M-2.0 Excd Vtniom 7.0 TX*120-Imr.ila 6T10*9 5:12 PU PS fi 3, M ** H l|| Hi li 1 !i< Si?S i|I !i?i?- p S !)! ! r |i !! r 88 j? l2 %1991f99f ri Il ^ ili ili iiiiiiii iii iii iiiiiiii i i i i l i 11111*33 il il f il I! i i l *1 II Lsa 1 P i!*K3p p fpii l i il P I iiiiiiii p pp ISS i l i ii iiii lit fllifi 111 lilil 8tP tPSilp3333 ^ir_-- v`f-Vi- -f$ PiiSSIjjji i l Bggig; I I ! S M ! 'iilSf.U Mi * 5333333333335355333333355555 33335353353535ZZ SzSi II II * i| r ! *r 3 3 3 ?3 555 535 335 553 Z I 1 1 U| ii 1 1 f S si HI Iiit | |I I sai sis sisaisil ili sSSSSSSl liP P P 888 pppppppp 88888888 53S3P?MiTl* Sl 'fp. ! ~ sp sp*- = f 'siti gg || Efpsss Ml IMi i i i i i i i II n II M.**1} : i Ii s: i s gS Si15 S 11i 3 3 1 1 *I K g|3* U K se s 11s i Z 1 1 < HcS "Si IlisSSIiassn m u 523 SSSSciSS P 8 P 8 P 8 88 8 S 3 2 3 II II i ili fil gmP P P p p p iiiiiiii P a P Ili gpSpSpSp cpip5p5Mi Ml IIIIIIII * IIMl * II II r &* * S i L i ii i 5gp u 2 5 3- SC i i1 i 1 1 sH1s i 1. r 1 3 1 1 3m S J| I3 z 1 1 Si=1 000456 000457 ---------- FA.------- .M20 U 2S-Day Oral Tox Study by Daily Gavage la Rala Slady; h o * * >l--t a f f a i SaM fcc M ttic McfboMcvbn: A aatytiealEqaipN tSyriaNaari battane* Somc/Vmbo: DricofExttactioarAaalyri: DatoAaayiu/Aatfym: Datea f Data RafeetWAaalyri: S a a p ltD iU TOX>120,Erphmtoiy 23-DayOralToxicityStadyby Da&yQ m |t fa Rata T-7023.T-7Q24, T-7022, T-7032, T*4293 RMLiver FACT-M-U A FAC44-2.0 R-SqaandVabe ' Maddka 041093, Amelia 062498, d Soap030199 AteLynl.1 Sope Y-aiattpL 3/22/99 RWW/SAH 0Z4/99, OSa1/99,03/14/99,0*2*9 HQjPMEEftttB 03*999,03/12/99.03/17/99.03/2499 DRB/KJH/HOJ S et A iuchacott RAT LIVER Graap Dw Method Btk Method BOt M rtrM k Mris Blk JC-250 R* <X^250r * C rm /4 Cr*4 30.0 Boif/day Racttvay I 14D m C reap4 30.0 e ifttty Recovery 2>2t D m C rup! lO.Omttyigy ma GroopS io .o i|k |io r Recover 1- 14D m Cm pS Recovery2-23 D m Creep 4 3.0m fftffrqr nos G m pt 3.0n*k^ey Recovery I -14 D m Creep 4 i.0m$/kt/f Recovery 2-23 D m -ph r Extractad Wi. S H20Blk~l K 20H M Rabbit Liver B ft-l Rabbit Liver Bfk-2 104F 106F llflF 110F I4SF 144F 147F I4IF 149F 190F 151F 1S2F 153F 194F 155F 157F I5SF 139F 141F 142F 143F 144F 145F 146F 147F (41F 149F 170F 171F 17P 174F 175F 177F 171F 179F IMF IflF II2F 113F IMF II5F IMF IC7P IS9F 190F 191F NA HA HA NA 0.9240 0.9240 &9 0.9242 0.3449 0.4113 0.4437 0.4699 04097 0.4416 03474 0.4341 0.1571 07221 0.1019 0 J1 II 03430 0.9194 0.9399 0,404 013107 0.4779 0.7719 0.4252 0.4732 0.4373 04394 0.7737 0l547I 0.1744 0.7937 0.4424 0.7352 0.4423 0l5442 0.3104 U7I04 04940 0.3512 0.3207 1.0370 0.3345 0.7563 01719 04832 09180 rr i C rib C w . afr <MDC <MDL MDL <MDL 253 250 49 99 144 118.7 02 130 102.7 103.0 150 11U 135 71.7 142 94.8 142 99.1 44.7 77.1 117.6 702 72.7 1207 903 45J 434 41.8 564 4M 115-9 34S9I1 333073 334730 333395 422128 404233 343202 325332 213147 247344 235351 132143 183230 201253 T itd A aw d arm s fr <MDL <MDL <MDL <MDL SM MH 23% 33% 0.U4 01137 00902 0130 01027 01030 0150 01114 00774 0135 00717 0142 00948 0142 00991 00447 00772 01174 00742 O07Z7 0121 00903 00459 00435 00418 00545 00435 0114 364 333 337 333 422 / * 343 325 218 243 235 112 133 203 A m asa FFOS afe <MDL <MDL 15% 28% OtlSS 00948 0140 00394 00571 00734 377 240 191 RS StODtVe <MDL <MDL 00304 0354 17. 0.0211 364 00350 24.3 00374 23.4 00212 234 00133 500 OQ36I 49 314 105 234 7.72 14.1 MethodDdectioa Limit(MDL); F F 0 3 -2 4 * 1 2 4 a 9 fr,r0 A A -1 2 4 artl - S P F H S - 3 ftM S D -50a tffrM * -S a ft FOAA Cafc-Caac hfr <MDL <MDC <MDL <MDL 219 247 223 173 0.00 ooo OQO ooo ooo ooo ooo 0.00 ooo ooo ooo 0.00 ooo ooo ooo ooo ooo ooo 000 ooo ooo ooo ooo ooo ooo ooo ooo ooo O.oo ooo 0.00 ooo 0.00 ooo Ooo ooo 0.00 OOO ooo ooo ooo ooo TatalA aaaat rroA A aefr <MDL <MOL <MDL <MDL 73% 39% 75% 53% <MDL <3401. <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <v4bL <MDL MDC <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <UDL <MDL <MDL <MDL <MDL <MDL Avana FOAA rt <MDL <MDL 81% 44% <MDL <MDL <MDL MDL <MDL <MDL <MDL <MDL <MDL N/A*Not Applicable FFOS-tatemoctaw FOAA-M aorooctiai Dria&actad/Aaalyri: DrieVcrifietfAttiljei: ta n tm .m n a m .ta n im .ta m .o m m lag 0698/99,06/0499 EA FFHS-F M S13-C9FI9000M413-CUF23COO- RSD StfoDtv. 44DL C alc.C aac aofr ,<UDL . <MDL 0199 f i '.tU D L -U ,, IM .. >;>*-193 *' 0254 M l* !^ ?v*-.-;i40, # = w a f m ot. <MDC , <MDL ? !V io i & * .* * .. . V & $ > * . :f M O ' i3 ao io o > ' i'M O -'-v . A .jM O ili # <MDL ^ ^ 0 7 v if- <UDL <MDL W lh m m ^^sOOO-j'-f^ ^ 0 0 ,0 1 ^ -7 ? ^ ftO O ;' L & t M : - ' 1- <MDL <MDL fe # !a o o .' 2&&040 </'; as|.o--<c <MDt ^ ^ roolvv a^t <MDL <MDL <MDL <MDL 41% 45% 41% 45% 0140 00309 0.1M 0428 1.19 <MDL 0491 040! 0.0143 0.0146 010115 0.00869 NR NR Wl NR NR NR NR NR NR NR NR NR NR NR NR NR U NR NR NR NR NR NR NR NR NR NR NR NR NR A <MDL <MDL 53% 53% RSD *M,Dv. <MDL <MDL 0454 0i454 0375 00145 0.00349 101 0477 114 000194 DWM 4DIV/M NR NR NR NR NR NR NR NR NR NR NR NR FACT-M-2.0 E w d V erioa 7.0 TOX.1204MMJt 1099 *12 FU 1 i 000458 2t-Dy O rai Tox Stndy by Daily Gavage la Rais Stady: Froda* N n to fr a l S ab a to *): M atrix: M adtod/Rcririoa: A n ljitie tlE p p w a ly tta N n k R ta n n a m i S aftw aa/V ariaa: Data o fExtrartiner/Aaalyc D ocefA aalyririA adyae Data a fData K aterioaM ariyac S a a ip fo D a ta TOX'!20lEapfentoty 2-0*yOraiToxidfySMy by DaDyG am e ia R iti T-7023, T-7024, T-7022. T-7012. T-6295 RM livar * rm iir Settinto riffe FACT-M-l.O* FACT-M-2.0 R-SqaaraJValeeSee A ttedano* Madrina 041090,Aatriia 061491, aadSaty 020199 Stop: * SccA itacfeM i M aaLynx3.t Y*fartoccpe SceAaachtfnti 2/22/99 RWW/SAH 02/2V99,03/1t/99,03/1699,05/2599 HOJ/MEE/DRB 03AV99,03/12/9, 03/17/99,05/2699 DRB/XJH/HQJ R A T L tV E R Cmp S aap ltf KxtndcdW t. I rti Daaa E O le. CMC. MetfaodBlk KMBlk-l 1*1 NA *<D L MctfaodBlk H20Bk-2 NA "*MDL Matrix BUt R iM iU w m n' NA <M)L M ani Bit Q C-Jw RAtfcU va BIk-2 I46F I06P NA 0.9240 09240 . :-MDL' 'xl**. r a s iv i QC-2M H* 1I0P 09242 1I0F 09242 Crea* 4 14F 03643 DUO * * * , I46F 04113 < M ***if' I47P 04457 I40F 04699 I49P 0.6097 ao/ ISO? 06416 'tM C rae*4 I51F 09476 ;V & 000 & 132F 0.6341 'v v ;O 0 0 -':> lilF 0.1576 ..oo 3 0 .0 n tty d a y t$4F 07221 Iceavov 1-14 D m 1S9F 0.MI9 M m W : C raaf 4 137F O liti 3 0 9 a tfttta r Recovery2-21 D m I9SF I39F 03430 09196 G rafi tO .O af'if/dej' K i r ..... 142F o .n 04004 E5m 100196 ma I63F 01107 94742 I64F 04779 91925 16SF 07719 116992 166F 04232 19141 I67F 04732 114702 IMF 06371 76152 G rafi tOLOas/kfVqr Recovery 1-14 D m M9F 170F I7IF 03394 07757 05671 393 169 226 C raff lO daf/kfU cy Xceaverv2 2* D m C rafl .0 m jkj * y 173F I74F I7SF 1771* I7SF 01766 07937 04626 o ith 04423 373 273 31.6 FFOS I79F 05462 IMF 00106 IIIF 07104 1I2F 05940 : .'0oqv I03F 01912 c OM IMF 01207 -- OOO G rafi 3.0mfkftay Raeavarv 1 14D m G rafi 3.0 ls*ay RacararyZ-Sf Deya 1I5F IMF 1I7F II9F I90P 191F 1.0570 01343 07560 00709 06002 09100 ooo V,.?AOOO y;-:. M #, S aiL B m - LhafQaantitana(LOQ): FOAA- 23 . t MadaodOrtarhaiItorti(MDL): FFOS-2J*t2_Sa*'*,FOA-l2Ja T attiA n-- t afFFHS e/ | MDL MDL MDL MDL 0% OS OK OS NR NO NR NR NR NR NR NR NR NR NR NR NR NR 4.6 to t 94.7 91.9 117 09.1 115 702 0393 0169 0226 .0372 00272 00316 US NR NR NR NR NR NR NR NR NR NR NR NR NR Dato Eafand/Aaalyat: Dato V oiBol/A aalyat: 02/26/99,03/10/99,0V 1 7 /9 9 ,03/22/9, OS/2 0006/99,06/09/99 BAD A vente FFBS rt <MDL MDL OS OK NR NR NR 97.1 0363 00320 NR NR NR RSD M513 S ii. Dar. Cale C ase. <MDL tft <MDL <MDL MDL MDL MDL #d v /o! fDIVAH 276 212 179 162 OOO OOO OOO OOO OOO OOO OOO NR OOO OOO OOO NR OOO OOO OOO NR OOO OOO OOO . OOO 0.00 OOO OOO 153 0.00 14.7 OOO 443 0116 OOO OOO OOO OOO 13.7 000502 OOO OOO 0 OOO OOO 0.00 OOO 0.00 OM NR OM OM OM NR 0.00 OM OM NR NRNetRcpofted OOO N /A -N atA ppfeaM a FTOS- F O A A * PcrflaonocUBO itt PFHSM513 C9F19COO- M6t3CtlF23COO* T atti A neeat afMS13 Fi <MDL MDL .' MDL MDL 92S 94% 60% 54% MDL MDL MDL MDL MDL OflX. MDL MDL mU . MDL MDL MDL MDL MDL MDL MDL <MDL MDL MDL MDL MDL MDL MDL MDL MDL MDL MDL MDL MDL MDL MDL ^ MDL MDL MDL MDL ' MDL MDL MDL MDL MDL MDL MDL A rante MS13 afe _ MDL MDL 93% 57% MDL MDL MDL MDL 4ID L MDL MDL MDL MDL BSD $14.Dar. MDL MDL 00205 0103. 40L MDL MDL MDL m d l MDL MDL MDL MDL M613 CafeCaoc. tfe MDL MDL MDL MDL 267 314 272 241 OOO OOO OOO OOO OOO OOO OOO OOO OOO OOO OOO OOO OOO OOO OOO OOO OOO OM OOO OM OM OM OM OOO OM OM OM OM &eo OOO OOO OOO OOO OM OM O.M OM OM OOO OOO OOO OM T etti Am avi afM613 ttfe MDL MDL MDL MDL 19% 105% 91% 11% MDL MDL MDL MDL MDL . MDL MDL <M>L MDL MDL MDL MDL MDL MDL MDL MDL MDL ` MDL MDL MDL MDL MDL MDL MDL MDL MDL MDL MDL MDL MDL MDL MDL MDL MDL MDL <M>L MDL MDL MDL MDL MDL MDL A vente M613 *fe MDL MDL 97% MS MDL MDL MDL MDL MDL MDL MDL MDL ' MDL RSD 814. Dav. MDL MDL 0161 0123 MDL 44DL MDL MDL <4DL MDL MDL MDL MDL FACT-M-2.0 Excd V aria 7.0 T O X -l204tar.iti 6/10/99 3:12 FM 000459 --------- i FA <*--+-otC-1 2 0 l-- a 2S-Day Oral Toz Study by Dally Gava{e la Rats hadiK (M ada(T (ttd(laaN )! M ak M abodUcviM : b aran e* SoftwareWcmoa; D aeofBUftctlw/Afra? DneaTAaalyatfAMlya: Datea f Dal RedBCtmfAaily: S ta p le D ata TOX-12R E q teao iy 2M )eyOnl ToxfcfcySttdy ly Da3yGsvagefa Rue T-7023, T.7Q24 T-7022, T.7Q32,T-6235 KMLiver m enane: FACT-M-l.Q* FACT-M-10 R-Sqeacd V ette M ediae 04109,Soap 020199 Rope: M wLynU Y ^M cqc Q4M/99 RWW0CMAK 04/2099, Q5/14A9.0S/2V99 HQI/DRB? P4/22/9R0V0S/99,05/11/99,05/26/99 KJH/MEE/DRB/HOJ RA T LIV ER C rap Deec H n l |tt 0 MnrixBtk 0 Q C .B O frk QC-M On* Q C -2b* C nepl Cosmi C rem i O.Onpli|/4oy Recovery I *14 Deve C respi # 0 .,* a ttq r Recovery 2-21 Deye C m pt 3 0 .0npt|ay Tdorecr Akshel C respi X .O s^ tfto y Recovery 1 14Dave G rasp* 30.0 *(/*/*? Recovery2 -2 f Deye C rw p) 3 0 .0 n g ftfttq r T rin irr Araytele G roaf) 3Q.0nt/kgfeey Recovery 1- 14Deyi G rafi M On^hfM m Recovery 2 2 t Deye S anplel H 20Kk-l H20 80^2 KjMit L ira Blk-1 RabW LiverKk-2 3M-MS 1M4ISD 6U-MS A U ISD 13M-MS U IM BD iU 2M 3M 4M 5M 4M 711 SM m 10M 11M I3M I4M I5M 17M ISM 19M 20M 2IM 22M 23M 24M 25M 2SM 27M DM 30M 3IM DM 34M 35M 36M 37M 3SM 39M 40M 4IM 42M 43M 4SM 46M 47M k rtn d id W l I 0.00 0.00 0.00 0.00 0.91! 0.9162 0.9091 0J09S 1.0701 1.0701 0.6511 9.6999 0.9162 0.6124 0.1920 0.909S 0.1965 0.1267 R6344 0.6972 0.1504 1.0701 0.9044 0.SS1I 1.0503 0.9993 04139 0.5331 0l7957 1.0663 0.7241 0.5990 0.56IS 0:7356 0.9176 0.9513 . 1.0SS5 0.9514 0.6419 0.6715 04SM 0.9225 049JJ #.574 017240 016670 1.0153 0.714] 0.9065 1.0667 04633 0.9711 nw Ci Jc-Cmc. Ik <MDL <MDL <MDL <MDL 274 2S6 319 300 2S9 291 Hi 129 102 124 104 13S 127 165 115 239 312 944 107 95.7 ' 4 " 404 39.7 36.4 34.6 254 194 294 319 26.0 254 444 93J 91.7 70.4 504 654 5S4 764 4S.7 H. 915 41.4 64J 494 59.7 511 . 56.6 T etti Aneaat efFFOS <MDL <MDL <m d I <MDL 92% 96% 107% 103% 97% 97% Oliti 0.129 0.102 0.124 0.104 0.131 0427 0.165 RI 15 0439 04119 R094 RIOT 0.096 R0S4S R04Q2 RQ397 R0966 R0346 R0259 ' R0192 R0290 R0329 0.0260 R0255 R0449 R093S R03I7 0.0704 R0509 . R0652 /0.Q5S0 R0762 R04I7 ROSO# R0925 55414 R0645 R0499 04597 R053I R0566 _ Average FFDS afe <MDL <MDL 94% 105% 97% RI33 0455 R099 0.0350 0.0211 R056I ROSTS 0.0SI9 RQS65 MeMedD e tta i link(M DL): fF O S -24m fcrO A A -Sm fem iS-24m fe.<S13-2SaadS0m fcM 613-25m fe DaeEnered/Aaaly*: Dale Vcrtfed/AaetyM: 05/05/9R05/2699 LAC M INM ,0fM IDEAD RSD Sti# Dev. <MDL <MDL 4% 4% 04 20 R03 474 0.1220 6.97 R0069 304 R0107 144 R604I6 574 R03272 224 ROI515 215 R0I17 5.W R0Q327 - M aa Ci R C mc. afe <MDL <MDL DTV/0I 6MVAM . 254 260 29943 31R30 344.99 31171 R00 R00 0.00 040 0.00 R00 0.00 040 RQO 0.00 RQO RQO RQO 0.00 5077 3415 1366 7910 4944 7045 5713 10045 4197 3712 2*73 14*9 1662 2026 6005 10321 1091 1559 1463 10095 7591 10021 4711 1545 3764 ttS7 SS7 1731 T ettiA m u* errOAA afe <MDL <MDL DIV/W DIV/M 15% 17% 100% 104% ' 115% 105% MDL <MDL <MDL <MDL . <KL <MDL <MDL <MDL <mdC <MDL <MDL <MDL <MDL MDL it 3.49 147 741 444 7.04 5.71 10.0 449 171 1S7 IJ9 L66 103 6.01 IR3 1.09 146 R46 10.1 749 10.0 4.7S 145 176 1.16 R II7 1.74 N /A -NrtAff& aNe .FTOSPOAA-PerfiaenoclanoMa FFHSF Msts*cmooo- M613 ClIF23COO- Average FOAA afe <MDL DTV/M 16% 102% 110% SDIV/N D1VAH DIV/M 159 349 1.76 . 164 136 146 RSD SU . Dev. <MDL 6DIV/M 2% 3% RIO 6DIV/QI HXVAN 6DIVAI 317 116 111 0.669 113 0434 17.1 US 494 145 344 0.435 C SbC ab ffe rat rat rat rat VALUE! fVALUEl 6VALUEI VALUE! VALUE! VALUEI (VALUEI VALUE! VAUIB VALUEI VALISI VALUE! VALUEI VALUE! VALUEI VALUE! VALUEI VaLi VALUE! VALUE! VALUE! VALUE! VALUE! VALUEI VALUEI VALUEI VALUEI VALUEI (VALUEI VALUEI VALUEI VALUE! VALUEI VALUEI (VALUEI VALUEI VALUE! VALUE! VALUE! VALUEI VALUE! VALUEI VALUEI VALUE! VALUE! VALUE! VALUE! VALISI T etti Aeeesat r a rt * rat rat rat NR rat rat rat rat rat rat ita rat rat rat rat rat H* NR NR rat rat ra t ra t ra t rat ra t ra t rat NR rat ra t rat rat NR NR NR NR NtaR ra t NR NR NR NR NR NR NR NR NR NR NR NR Average afe NR rat rat NR rat NR rat rat rat NR NR rat rat rat Ub SU. Dnr. NR NR rat rat rat rat rat rat NR rat NR rat rat NR FACT-M-2.0 B u d V cntta 7.0 T O X -12aW jtte ff!99 5:12 FM 000460 ----------- F A C ,- ___ . -1 2 0 ------------- *. 2S-D*y Oral Tox Study by Dally Cavate In Rata FrariaitN iak i(T q l Matrix: McAad/XctUsB AaatyrieM B oa fem tt S yitca N m to n IllW X M tio ftW W fV d lltK D rtcafE xfractiaa'A aal}: D ataafAaatyria/Aaaly: Data a fData E rria rtin a iA a riy f S ia p b Data TOX-1M , Exploratory Il-O a y O ral T a xfe ityS ttriyky D rily C avatala tota T.702J, T-7024, T-7022. T-7032.T-4295 MmUm F ilttm a r S c c to tia rifb t PACT-M-U * FACT-M-LO I-S g u n t Vata c Sea Attor ta l a M idrib 04109,S o * 02819 MmLynU S lept: Y4MaNfC S ttA s a d ttM i SetA ttaccatati 04AW9 RWW0CW5AH 04/20*9, 05/149,05/25/99 HOJ/DRB? 04/22/,o s jw n . e s /ii/t* w w n kjh/mee/drb/ho j RAT LIVER Creep Daaa fclwk^PIV 0 Matrix BOc 0 o c - io n * QC-MOb * QC-JKb * C raapl M aj/kfU ur Coeeal C raapl OOaf/fcfttay Oecevov t 14D m Craap t OAopfeptrisy Recovery2 *28 D m Craap 2 3 0 0 ajftffey T c to sA k to l C raapl M Aa^fciM ay lU tavav t 14D m C raapl 39B*kpUqr Recomy 2 2! Dayt C raapl M o a ito to TaleaiarAciytot C raapl R O agiaU qf Recavtrv l*14D m G raapl 390B f/k|toy Recovery2 21 D m la a p itl Estrattori WtT 1 H20BU-1 K30BJk>2 R attit LiverBik-I Ratok LiverBSk-2 3M-MSO 6MMS AMBD 12M-MS 13M-MSD tii 2M 3M 4M 5M <M 7M tM Ml I0M 1IM 13M MM ISM I7M ISM SMI 20M SIM 22M DM . 24M 2SM 2CM 2711 29M MM 31M llM StM ISM MM 37M 3SM MM 40M 4IM 42M 41M J 46M 47M DM 600 900 0.00 09K 2 0.9102 0.9091 0909 1.0701 1.0701 OASIS 0.4999 0.9142 0l4S24 0.8920 09090 OS94S 0.1247 0.C344 014972 0.IS04 1.0701 0.9044 08511 . l.ttSOl 09992 04*39 0.5331 07957 1.0642 01724 95990 Q.S41S 0.7354 0.917 99SI3 1.0055 0.9314 .48* 96715 OJSSO 99225 95915 0.5744 0.7240 0.4479 1.01S3 017143 0.9063 1.0647 03633 0.9711 rn u Calc. Caac> A iCMDL <MDL <MDL <MDL 273 2S4 219 211 247 291 49.0 96.6 49.7 50.9 1 54.7 40J 41.9 443 221 122 101 90.4 4M 34.4 45 SM 112.1 214 1U 12.0 29J 24J I4 J 22.8 244 44.1 21.1 444 S it 991 j / 417 $63 50.7 104 217 22.4 21.1 29.1 304 274 T atti A aeeat a rrm fe <MDL <MDL <MDL <MDL 91% SM 107% 104% 19% 97% 0 .0 M .......... 0.0964 0.0497 0.0509 0.0312 0.0547 00400 04> 00442 0221 0122 OlOS 00904 00419. 00344 00455 90514 O lii 00254 0.0284 00220 00299 00249 00149 0022 5 5 3 00441 00211 oo44 00531 00901 0.0453 00447 00541 00507 91038 00227 00234 00311 00298 0090 0027 Avarapa DUI n ft <MDL <MDL 88% 105% 93% 0054 0129 00190 00440 00255 08332 00663 0.0291 00293 W ftO D av. <MDL <MDL 7% 2% 90S 374 00204 0 00184 2I.C 00194 624 0021 402 00103 34.1 9 0 !! 309 00205 194 000559 142 0.00159 MJ1J Cric. Ciac, c^l <MDL <MDL <MDL <MDL 225 227 239J5 29340 217.83 247.4 900 900 900 0.00 0.00 900 OOO 0.00 OOO OOO OOO OOO OOO OOO 102 415 1485 2253 3155 2007 2021 2720 1491 224 1443 1844 1222 1475 2304 2001 1727 1775 1853 1234 1489 1428 788 1174 1270 492 969 741 Tatti Aawaal afM Sll P i <MDL <MDL <MDL <MDL fe% 74% 80% 98% 73% 90% <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL MDL <MDL <MDL <MDL <MDL MB 041 L4t 245 11 101 102 172 i.4 t 24 144 1.8 142 1.47 240 100 1.72 L7T MS 144 1.69 1.42 4 .H 1.17 1.27 0492 9969 974t A varila MSU alfe <MDL <MDL 76% 9% 81% <MDL <MDL <MDL Ut 1.73 . 142 1.78 LOI OIOI *b' 9tri.DVe <MDL <MDL 1% 20% 021 . <MDL MDL <MDL 460 087 266 0441 214 0321 174 0307 217 0455 184 0148 -- m *-- C ric Ciac. *fc <MDL <MDL <MDL <MDL 241 22 m* 21140 22541 23171 i OOO OOO OOO . OOO OOO OOO OOO 000 OOO OOO OOO OOO OOO 904 494 814 74.7 994 714 960 112 <14 11 142 113 164 11 S5 00 24 OOO OOO OOO OOO OOO OOO OOO 000 OOO OOO 800 M otoriDcttctioaLtoJl(MDL); W p S -li * /|,P O A A S ip fcm Doa EatcnrifAaalyat: Data V crifiO P Aaalyit: 0505/99.05/24/99 LAC O M W A O M M fE A D W A -N * Applicato wos- POAAITH 1 - frrflawTihnat M513 C9P19COO- M 6U -C U R 3 C O O . Votai AawaT" TM413 rt <M0L <MDL <MDL <MDL 1% 77% 43% 71% 76% 71% <MDL <MDL <MDL <MDL MDL <UDL <L <MDL <MDL MDL MDL <MDL MDL 4ID L 00904 00493 90834 00747 00995 00724 00940 0112 00416 0119 0142 0113 9006 O li MDL MDL 00422 <MDL <MDL <MDL <MDL <MDL MDL <MDL <MDL <MDL <MDL MDL A varila M413 MDL MDL 79% <7% 77% <MDL <MDL MDL 00172 0107 010 00622 MDL MDL USD StOPcv. <MDL <MDL 5% 12% 90S <MDL <MDL MDL 174 00150 384 00414 162 00172 IVA MDL <MDL PACT-M-2.0 Eacd V an ce TO TOX-120-Uvcr.xb tnwn 5:12 PM 000461 1 Fkrr-TVai-120 ' 2ft-Diy Oral Tox Stody by Daily Gavas la Rats FiodKtN aaboCftrt Sabetncc): Matrix: M cd w iM M Aanlyffcat EqufAcat SyOeaNoaba: Dateof EatactkMAoriyat: Dale o f AulyMMMlyiC DateofDate ftefectm'Aaelyat: S ia p te D a ta TOX1R Piptooney 2t-DeyOnJw k ity te d y fcyDxflyGavageh l t T-7Q23..T-70HT-7022,T.7032, T-6293 Rat liv er FCT-U-1.0A F CT-M-2.0 Madeihe 041099 Mm L M 04/1*99 RWW/7CMAH 04/20/99,0S/21/99,05/25/99 HQI/DRB/KJH7 s/oso* 04/9* w w meetcwh; R-SqeiradValac: Slop RAT LIVER Grasp te l Ceoc. U OtedUk Matrix Blk -JM H* Q C -250H * Q C -2* Crw p 4 H O m fkJd a y Creep 4 ) 0 .0 a |t|% ItooHii 1-14Dm C reap4 30.0sftU*y Recovery 2* 2t D m CreopS lO.OBgftg/dajr ma C rM ,S 10.0o p t9**T R oovor 1 14D m GroopS l* 0 fftfttap Recovery 2- 29 D m C reep X0mfk$Sty rros Creep 6 M ^W tgr Reeevov 1 H D m GreepO J.O m fltVtr R ccevay2-2ID m H20 Btt*t H2Bft~2 R ateU verB tel RebUlUvcr Btt-2 3M445 3M-MSD AUB KMSD 13M-MS 13M-MSD fU SOM SIM 52M S3M 54M SSM SOM S7M SSM S9M OIM C2M CM 45M 66M C7M M 09M 70M 7IM 72M 73M 74M 7SM 77M 7IM 79M I1M 92M <3M S4M SM 6M I7M IIM WM 90M 91M 93M MM 95M 0 *99 374.4500 310.0600 4001000 390.4100 379.4300 311.7500 NR NR HR NR NR NR NR NR NR NR NR NR NR NR 21.) 73. Nr NR NR NR NR NR 154 9*3 903 ii) IM m 24*9000 5001700 341.9500 429.1100 49*0600 4*9.7200 455.7600 403J500 32*9700 330.4600 26U200 209.1100 354.0S00 251.4300 MatedDcm(miUsa(ftffig: nOS-S*3*fcrOAA-2S*fc p ros p fo MMIm C atcC eac M ar tfe <MDC 1 MDL 1 MDL 1 <MDL 1 27409% 1 21575% 1 31931% I 30793% i 21104% 1 29090% VALUE! 1 VALUEI 1 VALUE! t VALUE! I VALUE! 1 VALUEI 1 VALUE! 1 VALUE! 1 VALUE! 1 VALUE! 1 VALUE! 1 VALUEI 1 VALUE! 1 VALUE! 1 J 1 731 1 VALUE! 1 VALUE! t VALUE! t VALUE! 1 VALUE! 1 VALUE! 1 153 1 9U 1 90. t 117 i IM t 1*0 1000 245630 1000 S0271C 1000 . 352337 1000 / 433347 1000 . 47(539 1000 49549 1000 456739 1000 400571 1000 5553 1000 332625 1000 27002*9 1000 1000 * 20790*7 253062.9 1000 250597.1 DateB attit^Aaaiyst: DeteVcrified/Aub*: <0/24/99, 03/1*99,<0/17/90,03/22/9. 05/24/9*05/24/99 LAC 06/01/9,06M 99 EAD Average O S rt <MDL <MDL 94% 105% 97% NR NR NR *0509 *114 *1053 419.4 3091 2371 USD SM. Dey. <MDL <MDL 4% 4% *0 *0 NR *0 NR *0 NR 2 *0317 301 *0344 2*9 *0261 2*44 95.73 lt.0 6 3*19 1*7 254 ' rOAA Cale. Ceoc. rt <MDL <MDL <MDL <MDL 254 260 299.93 31030 344.99 312.71 VLUfcl VALUE! VALUE! VALUE! VALUE! VALUE! VALUS! VALUE! VALUE! VALUE! VALUE! VAJfel VALUE! VALUE! *00 *00 VALUE! VALU VALUE! VALUE! VALUE! VALUE! *00 *00 VALUE! *00 0.00 0.00 VALUE! VALU VALU VALUE! VALU VALU VALU VALU VALUS VALU VALU VALU VALU VALU fetal A m w t fPOAA <MDL <MOL <MDL <MDL 5% 97% 100% 104% * 115% 105% NA NR NR NX NR NR NR NR NR NR NR Mr NR NR *00 *00 NR NR NR NR NR NR *00 *00 NR *00 *00 *00 Mr NR NR NR NR NR NR NR NR NR NR NR NR NR W A -N otA ppteaU e FFOS-PaftwoocteM FOA A " m fS-tafte Average FOAA rt <MDL <MDL 9% 102% 110% NR NR NR *00 *00 *00 NR NR NR D SM.te * . MDL <MDL *0232 *0340 * *0992 *00 NR *00 - NR *00 NR DIV/M *00 DIV/M *00 IXV/H *00 *00 NR *00 NR *00 NR te VALU VALUS VALU VALU VALU VALU VALU VALU VALU VALUS 4ot) 2433 2447 2703 903 2034 4347 5962 169 3*4 191 25.0 40J 1*3 VALU VALU VALU VALU VALUS VALU VALU VALU VALU VALU VALU VALU VALU VALU Va l VALU VALUS VALU valu VALU VALUE! VALU VALUE! VALU VALU VALU VALU VALU ______fe NR NR NR NR NR NR NR NR Mi NR 4.o 2.43 *43 2.70 *103 *03 415 SK *169 *0294 *191 *0250 *0405 .0,0103 rat NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR rat NR NR NR NR NR Mk NR rat Average Ma NR NR NR NR NX SD 8M.De*. NR NR NR NR NR *09 *12 0.0253 S tJ 119 6* *0940 5*7 *0151 0 NR NR *09 NR NR *00 rat NR *00 NR NR *00 NR NR *00 NR NR TOX-lW -tlvcrxli 0/1099 5:12 FM 000462 FACT-TOX-120 28-Day Oral Tox Stndy by Daily Gavage la Rats Sudy: frodart Ih rta r SrtMce): Marfz: . MdfcodflUvfafaa: Date o f ExOactioaMaatyil: D tfetfA adpbftailytf: ranflT ii ftintniinafftaityir S a a p k D ata TOX-I2R ExptortdTOX-121 Eaptamocy2-DayOralTaxkfy Sudyby DailyGavageJ*Rata 'T-7B23,T`7024, T-7D-7023, T-7024, T-7Q22, T-70J2, T-4295 R atL tar lU ttirar Sefiat lerigt* FACT4<1.0A FA<FACTM>1.0k PACT-M-IO R-Sund Vatw;Se*ABaefanoas H atrtinr 0*1034 M aidbc 0*1094 Mw Lj b M Mm L}d 3 J 04/1V99 RWW0CD4/HW9 RWW/3CP/SAH 04/2099. CcS/21/ML0V2D9R 03/21/99,05/25/99 HOJVDRMUH? 05/05/99,05/24/99,05/05/99,05/24/99, 05/24/99 MEEflUH/HQI RATUVER Craap 9m MahodBlk M rtriiBlk Q C -2pf* o c-:5 0 pp. Q C-SOp* C napl A ta |/k |U q r G rw p4 H O afftpttqr K tttw y 1 14D m GrM ?4 tt.O H fif'd ty Rceovcry 2 - 21 D m Cr* S IlO afftftfap FFHS GreapS ie.O B f/kfttajr te a v a r 1-14 D m Cfw pS lt.0 a |lk # lq r R*C9very2-2lDm m p^ 10*l[*tfy FPOS C r*M Zacevov 1 14D m Cmpl Xecovcry2 -2S D m Ifp ltl tOOBIk-I H20 Blk-2 RabMUyerBTT RaMtUverBlk-2 3M44S 3M-MSD M 44S SM*MSD u m -m s UM-MSD 49M 90M SIM 52M S3M 94M 55M 94M 57M SIM 59M IM 42M O4HM 4M 47M 404 49M 70M 7IM 72M 73M 74M 7SM 77M 704 79M iU 42M DM Mt$MM UH 47M MM 9M . 90M 91M 93M 4M 9SM PFOS CMC. *M 0 0 194 374.4500 2460400 4005000 390.4400 75355 391.7300 Vk HR NR NR NR rat NR NR NR NR NR NR NR NRJ 73.9 NR NR NR Mt NR NR 194 963 90.3 117 414 133 2469000 5012700 3411500 4211400 492.0600 499.7200 455.7400 403.3500 355585 3314400 2413200 209.1100 254.0900 251.4300 PFHS Cale. Cmc. tfe MDL MDL MDL <MDL 273 254 319 311 29.4i 29154 fVALUEl VALUS fVALUEl OVALUEI 9VALUBI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI mu 359107 243354 337434 345414 314441 223309 347000 49362 44349 47999 37903 42744 24199 fVALUEl OVALUEI VALUS OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI VALU OVALUEI OVALUEI ovaLi OVALUEI OVALUEI HrttoJTVirrrtna1Mil(MDL): PPOS-SA3aa'*90AA-25art.P TataJ AjMat efPFHS /k MDL <MDL <MDL MDL 9m 15% 107% 104% 19% 97% NR NR NR NR NR NR NR NR NR NR NR NR NR NR 340 359 243 334 344 316 223 347 . 49.4 414 410 37J 421124 Ml NR NR NR NR NR NR NR NR NR NR }*R NR NR A verti* PFHS tft MDL <MDL 19% 109% 93% NR NR NR 327 61.9 343 NR NR NR Detc Eaiered/Aaely: D*UVoilkd/AaaijM: 02/24/99,WW,ovnm, tamm,as 04/0499.069999 EAD RSD StlD ev. <MDL MDL 10723 10237 10930 NR NR NR 13.9 510 19.0 11.7 314 7.42 NR NR NR M513 CafeCaec. O i <MDL <MDL MDL <MDL 225 227 273.16 334.12 217.43 247.44 fVALUEl OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI oVaU OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI oVALUfi OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI TM IAm u I f M5U a'i <HDL MDL <MDL MDL 75% 74% ' .91% 112% 73% 90% U& NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NR NkR NR NR NR NR NR NR NR NR NR NR NR NR NR Avcraga M513 4fr MDL MDL 70% 102% 41% NR NR NR NR NR NR NR NR NR N/A-NMApptfcaMa FFOS*FcrfhBiooetne 70AA- USD 4(4. Dev. MDL MDL m 30% 131 NR NR NR NR NR NR NR NR NR M413 Cale. CMC rt MDL MDL MDL MDL 241 229 147 313 325.91 23171 fVALUEl OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI OVALUEI VALUS VALUS VALUS VALUS VALUE! VALUS VALUS VALUS VALUS VALU VALUE! VALUS VALUS VALUS VALUS VALUS VALUS VALUS VALUS VALUS VALUS VALUS VALUS VALUE! VALUS VALUS VALUS VALUS VALUS VALUS VALUS VALUS VALUS VALUS Ti M Am u I ' MM413 afe <MDL <MDL <MDL MDL 4t% 77% 43% 71% 74% 71% ta NR NR NR NR NR NR NR NR NR NR kR NR ` NR ft NR NR NR NR NR NR NR NR .NR NR NR NR NR NR NR NR NR NR NR NR NR NX NR NR NR NR NR Average M413 MDL MDL 79% 47% 77% NR NR NR NR NR NR NR NR NR RSD SM.DCV. MDL <MDL 9% 13% 103 NR NR NR rat NR NR NR NR NR FAC-M -2.0 E u d Venta* 7.0 TOXI20-tivcrjs 4/1099 9:12 PM 3M Environmental Lab *Fluorine Analytical Chemistry Team P F S 's PFHS perfluorohexanesulfonate C6F13S03- PFOS perfluorooctanesulfonate C8F17S03- PFOSA C8F17S02NH2 PFOSAA C8F17S02N((CH2CH3)(CH2C00))- M556 . C8F17S02N((H)(CH2C00))- M570 C8F17S02N((CH3)(CH2C00))- PFOSEA perfluorooctanesulfonylethyl amide C8F17S02N((CH2CH3)(H)) Et-FOSE-OH PFDS perfluorodecanesulfonate C8F17S02N((CH2CH3)(CH2CH20H)) C10F21SO3-** PFCA*s POAA M513 M613 M463 M563 M363 perfluorooctanoate perfluorodecanoate perfluorododecanoate C7F15COOC9F19COOC11F23COOC8F17COO- ** C10F21COO- ** C6F13COO- ** PFS = perfluorinated sulfoante PFCA = perfluorinated carboxylic add ** no standard material available for confirmation; 000463 3M Confidential - Attomey/Client Work Product Privileged - D o N ot Disclose PFHS in M ale and Fem ale R at Liver, Group 5 3M Environmental Lab - Fluorine Analytical Chemistry co ! i 0 "5 PFOS In M ale and Fem ale R at Liver, Group 6 3M Environmental Lab - Fluorine Analytical Chemistry UU0464 POAA in Male and Fem ale R at Liver, Group 2 3M Environmental Lab - Fluorine Analytical Chemistry 1 14 28 Day 10 9 6o 7? 6 t5 S E 4o 3 a w 2S 1 0 M513 in Male and Female R at Liver, Group 2 3M Environmental Lab - Fluorine Analytical Chemistry Team, Project: FACT-TOX120 3 Ie 2.5 2I 8 c <3 1.5 o I 1* 0.5S 4 /ft 1 14 28 Day M613 in Male and Female R at Liver, Group 2 3M Environmental Lab - Fluorine Analytical Chemistry Day 0.16 0.14 0.121 0.1 I 0.08 0.06 0 0 .0 421s 0.02 0 00465 D 000466 000467 TOX-120,35M G3 060899009 100-, M613 (C11EZ3CQCE)1 3: MRM o f 1 Channel ES5.85 TIC 1.09e3 % 0.69.Q.75 23 ` v * 0650899009 lOO-i 1.72^2.13^ \2 - 5 8 \3 -3 1 3.85 4-^ 4 .8 8 f ' \ 5,59^ 1 6.06 |M63 (C1UKZ100CE]| 5.72 6.89 7.7U 7.86 / r m 6:i^RM o f ihannel ESTIC 559 % 0 38 1 03 1-47i^^.11,.5599 3 77 536 22..6655 33..0099 33..55.3S /s 44..8866 55..2255.. | 54 11i*i 11111f i i*i -,06089900? 100 ^ 1^ 11 hfyfa* ,W | 4 , , r , u v ^ |M513 (C9h l9C O O ^ 6.75 7.52_ 8 .14.8.29 ,, 7.02 \ .^ 1 C s '? '61 2: MRM o f 1 Channel ESTIC 8.68e3 %. 060899009 100-, ' 'i t t 1 1 1 1 1 i 1 i , - i 1 1 i i i i 1 i i 1 1 1 i 1 rv~[~ |M36'3"(C8FI'KXKFJj %: 1 1 1 1 1 1 j 1 1 r i i"T 1 1 1 j '1r,,v i "i r 1 1 I 1 1 1 1- 5: MRM o f 1 Channel ES TIC 6.65e3 060899004' " ' 100-, %- (PO A A fC 7H 5C O O -l Tn ' ' 111M H l"r" 5.14 1: M R M o f 1 C hannel EST IC 1 .5 6 e 5 m "t r f r r i r1 1 060899009 100-, 1 ................................................................ ..C h a n n e l E S - M3&3 (C6E13UUU-)| TIC 489 0.66 1-08 1-64 8.93 Time 000468 000469 000471 000472 ; Environmental Laboratory O m RequestForm . . 3M Environmental Laboratory 935 Bush Ave. Building 2-3E-09- St. Paul, MN 55106 Attn: Sample Custodian Phone (612) 778-6750 Fax (612) 778-6176 SafelyConcerns/SpecialHandl ing. [P.rmpm . ., v / V jagafeas^ >>*1Cffl^i*VSri* WWfeKgj :' f-A /Sample No. (Range 0-999)' [llab AequestNo.' I I Data Received PlojaaLaad----------------- Expected Completion Data k in Planning Status O D /n x /n n Quality Review * 10 Class/Pflority Date Shipped 1M&.IPaSSfe >: T^ J 'i-ii, - is s m . ,0 3 / / :/V/ ... '' .:?***'?* .. . . -. -V--v--. -" ;-------------'-.--:- VC--.'.. / sg i ', > *.'. v.* v . r " --"J *. , hi *" ,`k.r * . .. ' ...... . V ' ^ *. -a v :' .V;5; . T~ " : . r^ `. " :.;v; i`?.>:;-/V;''T `." * :..>.\.;' .'. r . I.'. V* tt'' I 'JW `^ -!y -;^ T --J/;/yJ-V*1/ CV: '!V' - v i * - . p - . - .- * --- .'*:t; r.", .'i.' ./'.'.A'/lv'-V/'-''.-.'. '-vA-fj' . . ' / .f .. i. , . . . , - - ' . . r.-: K v : . j;.r .; . -.V c v` ' : v .t*... ;... y . ' ------ :-------------i,-- Total Container^ of Each Item O 000473 C hain of C ustody R ecord 3M Environm ental Laboratory b v ' Forni 35176-PWO 3M Facility , Address 3 /0 :: '1 ' ,. . 1 .`j i- ,1. 1 ` T n y i f n l 0Ci\\ vJJ ' , ' ' 1;.. . City. State. Zip Code _________ S\. P f i J ,,h : - ,ff| lHlG MA) S S M - .. y bi V lQ 7 lW ' U O ( -L b 3M Requester _ f . . . . . . . . va V . '* , rlO n /in 3M Project Lead - A ' ' ( .<;/> ` i vV; : t ' ' ' 1. . : . ' 3MProJectTitle , ,. |. JOTnv .0W :Km TA X ISO ,).?/>.. Ar/.l TDtf P f i 3M Facility Contact . ' U :,:i; : HiM.-.* r j u *:V ' ' n .*'****': ' '-i..*..? 0`i? Hi 3MTelephone Number 3M'ProJect Number. , .. . ie.JPz.4i / Rocu^nn 3M Department Numtier : qa< ' ' ' - Lab Requesl/Template Number ________________ . 7 3 V - S I n . ____ SampledBy(Print) SamplerSignature V IA '' " Contractor<,/..if.f..w...f..1../.,....*......;..., :1 tin r x Dele Number Containers -, of each Preservatives f ( 3 K Sam ples S p lit See A ttachm ent : Comments Item # K) A '!. - ' . I Sample Description . !S A w /W Date Time Matrix 8i Mi i N Xz t' X 9z i i tlf- ' 1 G lA ^ ^ o O ^ (!iiiiT i) ! VniliVilc.!rl u p n n " ' i r i m ' p i f i * rPTfijl) S f l t l- 0 c iv Fil S j } f f tsp in l i t i ' 1' 4tSr` 1 f,,F I 2 G ro2 L iO A r L ii/tr 18 , t ,* t' ' t* iO l U jO f.H. f : . w: iler-iLfr irt-Tortna v-v, I.i-.I . 34 1 4 .i L-:Ji! 1 \rtr L ivtr 1 . t t r-liili 9 l i L'il i>; ir 1 M h ih s - 5 -C xji 6 (I r p L Lii/vr Ln/-rr 18 If" 1;.IO j h iIC 'iri'.:! .j ' i 7 ....... ________________________ -- ------------------ -- -------------------------- -- T 8 9 . . . * ' 1 ' * ** 10 Vi / 4 i : . i-H i ' t . * * 11 12 13 -- :----------------- ~ ------- :-------- -------------------------------------- ------------ Item # Relinquished By/Affiliation Time Date Shipped Via Received By/Affiliation Time Date J r Bvprt-M . lM - J __CJh a m *____ 2 L m j L 0 2 l n ? h f'l: !:' ;Oin I a lli. fi ui BESTCOPjTCMIWjLr Original - Accompanying Samples Last Page Orlgnalor See Reverse Side For instructions Total Containers of Each Item 000474 C hain o f C ustody R ecord 3M Environmental Laboratory Forni 35178-PWO 3M Facility 3 ft) Tovrc.^locioi Address (J O 3 2 -3 .E -0 1 City, Stale. Zip Cod _____ S i, Paul, MM S S I3 3 nq71Pf U o i J, 0 SMRequeKer 3M ProjectLead M ri/n C .& s*. 3Mpro`#c,Ti"# .. __________ K r i Hn5*____________________ T W . 3M Project Number WOToy 3M Fadty Contact TfcXiao 2SCV 5 rJ *n>y YPSs I r R ii+j R V qaqiiopo/B U ^ qi^o 3M Department Number Mctrvh C a s e , 3M Telephone Number HM l Lab Requeat/Template Number _________ __ ______________ 7 3 3 - S I ; ) ________________________________________ Sampled By (Print) Sampler Signature Item # 1 TGir-I 2 G rp 3. 3 4f & p*t 5 6 Grp L 7 8 9 V /A . h )lA Sample Description Contractor A )0T O * Dato ll/o lM - I3 I r t h s Date Time Matrix L iter Lit/tr / .itor L lW LiVer Liw r _4r-- Number Containers of each Preservatives 2 n O Z 8M X XX Sam ples S p lit See Attachm ent Comments (jnA\h AV 1 IfVnviii nlt/foyx iJhhn ^Arrin/i> tRr/jpV S i t 38 r 28 28 S p ttim e n Irsi 4t)r r n*HtrrWr .motormff1h,hK Ur. p o ifo q at . ------------ ;----------------------- -- ------------------------------------------ * 10 / 11 *w 12 13 -- Item # UL Relinquished By/Afflliation Time Date Shipped Via Received By/Affiliation k X ^ n e . B t f n j i f i h k C JjL nv* 7T- ' -'i; Time h. Date t i v i * v y t aetPana-rinnator ,r\ ' ' . - f~! ' I. r> f ? : * > n< , f \' See Reverse Side For Instructions 000475 11/09 'a 18:24 FAX 01736418343 NOTOX B.V. @003/017 1 I ] 3 PROTOCOL 1 I j EXPLORATORY 28-DAY ORAL TOXICITY STUDY ' WITH | TELOMER ALCOHOL, TELOMER ACRYLATE, PFHS AMD PFOS (positive control) ! BY DAILY GAVAGE | IN THE RAT * FOLLOWED BY A 14/28-DAY RECOVERY PERIOD J J NOTOX Project 242933 NOTOX Substances 83484, 83493. 83502, 84456 and 84141 j 3M Test No. T-7023. T-7024, T-7022. T-7032, T-6295 j - page 1 of 16 - J 000476 t 11/09 *98 16:24 FAX 31736418543 NOTOX B.V. 0004/017 TELOMER ALCOHOL/TELOMER ACRYLATE/ /PFHS/PFOS NOTOX Project 242933 l 3M Test No. T-7023, T-7024 I T-7022, T-7032, T-6295 ! PROTOCOL APPROVAL 1 ----------- :------5------- 1------------------- STUDY DIRECTOR : 1 Ir. S.C.M. de Hoog . Date: 11 JELopfcorn-bOe 1 Q 0 ( 9 | SPONSOR: J 1 J ] Marvin T. Case, DVM, PhD Corporate Scientist SM Toxicology Services D*t,: iv J ti iU * I f f f . L. c 'I * Page 2 - 000477 11/09 '95 18:25 FAX 31738413543 NOTOX B . V . 1 TELOMER ALCOHOL/TELOMER ACRYLATE/ /PFHS/PFOS 0005/017 NOTOX Project 242933 1 PREFACE ] Sponsor 1 Study Monitor 1 Invoice Contact Testing Facility Study Director J Pathology 1 ] SM Toxicology Services 3M Center, Bldg 220-2E-02 St. Paul. MN 55144-1000 USA Marvin T. Case, DVM, PhD 3M Toxicology Services 3M Center, Bldg 220-2E-02 Telephone (651)- 733-5180 Fax (651)- 733-1773 Barbara Nelson 3M Procurement Operations 3M Center. Bldg 224-1N-04 St. Paul. MN 55144-1000 Telephone (651)- 733-0766 Fax (651)- 733-1799 NOTOX B.V. Hambakenweterlng 3 5231 DD 's-Hertogenbosch The Netherlands Ir. S.C.M. de Hoog Dr. J. Th. Wilson .V - Page 3 - 000478 11/09 '96 16:25 FAI 31736416543 NOTO! B . V . 1____________________________________________ ____ 1 ! TELOKER ALCOHOL/TELOHERACRYLATE/ /PFHS/PFOS 0008/017 NOTOXProject 242933 STUDY PLAN 1 Start of Treatment ] 06 October 1998 (males)' 08 October 1998 (females) Start Recovery 1 04 November 1998 (males) 06 November 1998 (females) Blood sampling 1 03 November 1998 (Main groups, males) 04 November 1998 (Main and Recovery groups 1 and 2, males) 05 November 1998 (Main groups, females) 06 November 1998 (Main and Recovery groups 1 and 2, females) 18 November 1998 (Recovery groups 1, males) 20 November 1998 (Recovery groups 1, females) 02 December 1998 (Recovery groups 2, males) 04 December 1998 (Recovery groups 2, females) Urine collection predose 29*30 September 1998 (Recovery groups 1 and 2) day 7 11-12 October 1998 (Recovery groups 1 and 2, males) day 7 13-14 October 1998 (Recovery groups 1 and 2, females) J day 14 18-19 October 1998 (Recovery groups 1 and 2, males) day 14 ; 20*21 October 1998 (Recovery groups 1 and 2, females) end of treatment : 03*04 November 1998 (Recovery groups 1 and 2, males) end of treatment : 05*06 November 1998 (Recovery groups 1 and 2, females) end of recovery : 17-18 November 1998 (Recovery groups l, males) ] end of recovery end of recovery 19-20 November 1998 (Recovery groups 1, females) 01-02 December 1998 (Recovery groups 2, males) end of recovery 03*04 December 1998 (Recovery grdups 2, females) ] Necropsy 03 November 1998 (Main groups, males) 04 November 1998 (Main groups, males) 05 November 1998 (Main groups, females) 06 November 1998 (Main groups, females) 18 November 1998 (Recovery groups 1, males) 20 November 1998 (Recovery groups 1, females) 02 December 1998 (Recovery groups 2, males) 04 December 1998 (Recovery groups 2, females) Draft Report ] 26 March 1999 I 000479 Pag 4 - 11/09 '98 18:25 FAX 31736418543 l NOTO* B . V. 0007/017 TELOMER ALCOHOL/TELOWR ACRYLATE/ /PFHS/PFOS 1 NOTOX Project 242933 TEST SUBSTANCES The sponsor 1s responsible for the completeness of all test substance data. All available Information on characteristics of the test substance will be taken Into account before start of the study 1n order to determine 1f they conflict w1th/m1ght affect the proceeding of the study. ] NOTOX SUBSTANCE 83484 (data will be added by protocol amendment) Identification TELOMER ALCOHOL (T-7023) 1 Description Batch Purity Test substance storage 1 Stability under storage conditions Stable Expiry date Stability in vehicle 1% aqueous carboxymethyl cellulose: not indicated r Safety precautions Corn oil: not Indicated Gloves, goggles and face mask to ensure personnel health and safety Disposal Category NOTOX SUBSTANCE 83493 (data will be added by protocol amendment) Identification TELOMER ACRYLATE (T-7024) Description Batch J Purity Test substance storage Stability under storage conditions Stable 3 Expiry date Stability 1n vehicle 1% aqueous carboxymethyl cellulose: not indicated Corn oil: not Indicated .x Safety precautions Gloves, goggles and face mask to ensure personnel health and safety ] Disposal Category J - Page 5 - 000480 11/09 '99 16:28 FAX 31736418543 NOTOX B.V. @008/017 TELOMER ALCOHOL/TELOMER ACRYLATE/' /PFHS/PFOS NOTOX Project 242933 NOTOX SUBSTANCE 83502 (data will be added by protocol amendment) ] Identification Description Batch (T-7022) Purity ] Test substance storage Stability under storage conditions Stable Expiry date ] Stability 1n vehicle Safety precautions 1% aqueous carboxymethyl cellulose: not Indicated Corn oil: not Indicated Gloves, goggles and faee mask to ensure personnel health and safety Disposal Category NOTOX SUBSTANCE 84456 (data will be added by protocol amendment) Identification PFHS (T-7032) Description Batch Purity Test substance storage Stability under storage conditions Stable Expiry date Stability 1n vehicle 1% aqueous carboxymethyl cellulose: not Indicated Corn oil: not indicated Safety precautions Gloves, goggles and face mask to ensure personnel J Disposal Category health and safety 1 NOTOX SUBSTANCE 84141 (data will be added by protocol amendment) Identification PFOS (T-62P5) J Description Batch Purity Test substance storage Stability under storage conditions Stable Expiry date Stability in vehicle 1% aqueous carboxymethyl cellulose: not Indicated Corn oil: not Indicated Safety precautions Gloves, goggles and face mask to ensure personnel health and safety Disposal Category ] Vehicle 1% aqueous carboxymethyl cellulose or Corn oil, specific gravity 0.92 Rationale for vehicle Stability 1n vehicle Based on trial formulations performed at NOTOX Stability over 4 hours will be determined by the * sponsor - Page 6 - 0C0481 L___:________ ,_________ __11/09 *93 18:26 FA* 31736418543 NOTO! B.V. 1 , TELONER ALCOHOL/TELOMER ACRYLATE/ /PFHS/PFOS 009/017 NOTOX Project 242933 TEST SUBSTANCE FORMULATION Method Storage conditions Formulations (w/w) will be prepared dally within 4 hours prior to dosing. Zf necessary, adjustment will be made for specific gravity of vehicle. At ambient temperature No chemical analysis of dose preparations will be performed. PURPOSE AND RATIONALE The nature and purpose of this exploratory study will be to determine and compare the relative oral toxicity in rats following oral (gastric gavage) doses administered daily over 28 days and identify developmental compounds of lesser toxicity for commercial development. This study should provide part of a rational basis for toxicological risk assessment 1n man. The oral route was selected as 1t 1s a possible route of human exposure during manufacture, handling or use of the test substance. GUIDELINES This protocol was reviewed and agreed by the Article 14-functionary and the Ethical Committee of NOTOX as required by the Dutch Act on Animal Experimentation. The study procedures described 1n this protocol will be based on the following guidelines: 1) EC Directive 96/S4/EEC, Annex IV.D. replacing EEC Directive 67/548/EEC, Part B : Methods for the Determination of Toxicity and other"Health Effects; B.7: 'Repeated Dose (28 days) Toxicity (oral)". Official Journal of the European Communities -No. L248, September 1996. 2) OECD Guideline for Testing of Chemicals, Guideline 407: 'Repeated Dose 28-day Oral Toxicity Study 1n Rodents', Paris Cedex, 27 July 1995 This protocol, study procedures and the report will not be Inspected by the NOTOX Quality Assurance Unit. ARCHIVING NOTOX B.V.. will archive the following data for at least 10 years: protocol, raw data, report and all specimens. No data will be withdrawn without the sponsor's written consent. - Page 7 - 000482 11/08 '98 18:27 FAI 31738418543 NOTO! B.V. 1 _______________________________ ___ TELOMER ALCOHOL/TELOMER ACRYLATE/ /PFHS/PFOS I 010/017 NOTOX Project 242933 TEST SYSTEM ] Test System ] Sprague Cawley rat Cr1:CD BR, outbred, SPF quality. Recognised by International guidelines as the recommended test system (e.g. EPA, FDA, OECD, EEC). Females will be nulUparous and non-pregnant. Source : Charles River, Sulzfeld, Germany Age at Start of Treatment Approximately 6 weeks 1 Number of animals 84 males, 84 females Randomisation 1 At least 5 days before study start, by computergenerated random algorithm according to body weight, with all animals within 20% of the sex mean. A health inspection will be performed prior to commencement of treatment to ensure that the animals are 1n a good state of health. ! Identification Earmark and tattoo ALLOCATION ] ] Group Identification Test Substance Number of animals Animal numbers males females males females J 1 Main group Vehicle control 1 Recovery group 1 Vehicle control 1 Recovery group 2 Vehicle control 88 33 33 1- 8 ! 97-104 9-11 105-107 13-15 109-111 2 Main group Telomer Alcohol 88 17-24 113-120 2 Recovery group 1 Telomer Alcohol 33 25-27 121-123 1 2 Recovery group 2 Telomer Alcohol 3 Main group Telomer Acrylate 33 8 29-31 125-127 33-40 129-136 3 Recovery group-1 Telomer Acrylate 33 41-43 137-139 3 Recovery .group 2 Telomer Acrylate 33 45-47 141-143 ] 4 Main group 4 Recovery group 1 88 33 49-56 145-152 57-59 153-155 4 Recovery group 2 33 61-63 157-159 5 Main group PFHS 88 65-72 161-168 5 Recovery group 1 PFHS. 33 73-75 169-171 5 Recovery group 2 PFHS 3. 3 77-79 173-175 6 Main group PFOS (positive control) 8 8 81-88 177-184 ! i 6 Recovery group 1 PFOS (positive control) 3 6 Recovery group 2 PFOS (positive control) 3 3 3 89-91 185-187 93-95 189-191 I Test substances Telomer Alcohol (substance 83484), Telomer Acrylate (substance ( 83493) and (substance 83502) to be tested at a dose level of 30 mg/kg body 1 weight/day. PFHS (substance 84456) to be tested at a dose level of io mg/kg body welght/day. PFOS (substance 84141) to be tested at a dose level of 3 mg/kg body welght/day. - Page 8 - 000483 11/09 '93 18:27 Fa * 31738418543 1 NOTO! B . V. TELOMER ALCOHOLfTELOHER ACRYLATE/ /PFHS/PFOS 0011/017 NOTOX Project 242933 ANIMAL HUSBANDRY Conditions Air-conditioned room with approximately 15 air changes per hour and controlled environment with optimal Conditions being a temperature of 21 3*C and a relative humidity of 30*70%. Lighting will be 12 hours artificial fluorescent light and 12 hours dark per day. Accommodation Group housing of 3*4 animals per sex per cage 1n stainless steel suspended cages with wire mesh floors. Acclimatisation period 1s at least 5 days before start of treatment under laboratory conditions. Diet Free access to standard pelleted laboratory animal diet (from Carfll Quality BVBAr.Oud-Turnhout, Belgium). Each batch will be analysed for nutrients and contaminants are analysed on a regular basis. Results are examined and archived. Water Free access to tap-water. Certificates of analysis (performed quarterly) are examined and archived. TREATMENT Method Frequency Dose volume Dose level Oral gavage, using a stainless steel stomach tube. Formulations will be placed on a magnetic stirrer during dosing. f Once dally for at least 28 days, approximately the same time each day, 7 days per week. Main group animals are dosed up to the day prior to necropsy. 5 ml/kg body weight. Actual dose volumes will be calculated weekly according to the latest body weight. Group 1: 0 mg/kg b.w./day (Vehicle Control) Group 2: 30 mg/kg b.w./day (Telomer Alcohol) Group 3: 30 mg/kg b.w./day (Telomer Acrylate) Group 4: 30 mg/kg b.w./day Group 5: 10 mg/kg b.w./day (PFHS) Group 6: 3 mg/kg b.w./day (PFOS, positive control) RECOVERY Duration Recovery group 1: at least 14 days Recovery group 2: at least 28 days i- - Page 9 - 000484 1 1 / 0 9 '9 8 1 8 : 2 8 F A X 31738418543 NOTO! B.V. 1 _____________________ I TELOMER ALCOHOL/TELOMER ACRYLATE/ /PFHS/PFOS 0012/017 NOTOX Project 242933 OBSERVATIONS 1 Mortality / Viability 3 Clinical signs 1 1 Body Weights ]. Food consumption Water consumption Twice dally. Animals showing pain, distress or discomfort, which 1s considered not transient 1n nature or 1s likely to become more severe, w111.be sacrificed for humane reasons. The time of death will be recorded as precisely as possible. Twice dally, detailed clinical observations will be made 1n all animals: once Immediately after dosing and once approximately 4 hours after dosing. The time of onset, degree and duration will be recorded. All symptoms will be recorded and graded according to fixed scales (specified 1n the report). Treatment period : on days 1, 5, 8, 12, 15, 19. 22, 25 and 28. Recovery period : on days l, 5, 8, 12, 14, 19, 22, 25 and 28. Weekly. Subjective appraisal will be maintained during the study and a quantitative assessment Introduced 1n the event of a suspected treatment related effect. CLINICAL LABORATORY INVESTIGATIONS (Main and Recovery group animals) t J Blood samples will be collected under light ether anaesthesia, between 7.30 and 9.30 a.m. Immediately prior to post mortem examination for Main and Recovery group animals, and for Recovery group animals also at the end of the treatment 3 period. The animals will be fasted overnight (with a maximum of 20 hours) before blood sampling, but water will be provided. Blood samples will be drawn from the retro-orbital sinus of all Main and Recovery rats/sex/group and collected Into tubes prepared with EDTA for haematologlcal parameters (0.6 ml), with citrate ] for clotting tests (1.0 ml) and untreated tubes for clinical biochemistry parameters (>2.0 ml). ! - Page 10 - 000485 11/09 '98 16:28 FAX 31736418543 1l"... . .......... . NOTOX B.V. ---- -- 013/017 TELOMER ALCOHOL/TELOMER ACRYLATE/ /PFHS/PFOS 1 NOTOX Project 242933 ! HAEMATOLOGY 1 The following haematology parameters will be determined from blood prepared with EDTA as an anti-coagulant, using the Instruments listed: Parameter Unit ] Erythrocyte count T/l Instrumentation Sysmex K-1000 1 Haemoglobin Haematocrlt mmol/I 1/1 Sysmex K-1000 'Sysmex K-1000 1 Mean corpuscular volume fl Sysmex K-1000. Mean corpuscular haemoglobin fmol Sysmex K-1000 Mean corpuscular mmol/1 haemoglobin concen i tration Sysmex K-1000 * Platelet count G/1 Sysmex K-1000 Red cell distribution width % Sysmex K-1000 Total leucocyte count G/1 J Differential leucocyte l(rel) count Sysmex K-1000 Manual (Microscope) I The following haematology -parameters will be determined, from blood prepared with citrate as an anti-coagulant, using the Instruments listed: 3 Parameter Unit Prothrombin time sec Instrumentation Sysmex CA-5000 Partial thromboplastin time sec Sysmex CA-5000 j Page 11 - 000486 11/09 '98 16:29 FAX 31738413543 1 1 -- - - ' -- NOTO* B.V. 014/017 1 Telomer alcohol/TELOMER ACRYLATE/ /PFHS/PFOS 1 NOTOX Project 242933 I CLINICAL BIOCHEMISTRY The following clinical biochemistry parameters will be determined from serum 1 samples using the instruments listed: Parameter ' Unit Instrumentation ] Alanine aminotrans pkat/1 ferase 1 Aspartate aminotrans (ikat/1 ferase Bilirubin, total pmol/1 Cholesterol, total mmol/1 Triglycerides l Creatinine mmol/1 pmol/1 Glucose mmol/1 Urea mmol/1 Protein, total fl/1 Protein, albumin g/i J Protein, globulin g/l Albumin Globulin ratio 1 Alkaline phosphatase pkat/1 : Sodium mmol/1 Potassium ] Chloride mmol/1 mmol/1 Calcium mmol/1 Phosphorus mmol/1 Epos selective analyser 5060 (Eppendorf) Epos selective analyser 5060 (Eppendorf) Epos selective analyser 5060 (Eppendorf) Epos selective analyser 5060 (Eppendorf) Epos selective analyser 5060 (Eppendorf) Epos selective analyser 5060 (Eppendorf) Epos selective analyser 5060 (Eppendorf) Epos selective analyser 5060 (Eppendorf) Epos selective analyser 5060 (Eppendorf) Epos selective analyser 5060 (Eppendorf) Calculation {Protein total - Albumin] Calculation {A1bum1n/G1obul1n] Epos selective analyser 5060 (Eppendorf) EFIX 5055 Flame Photometer (Eppendorf) EFIX 5055 Flame Photometer (Eppendorf) Jenway PCLM3 EFIX 5055 Flame Photometer (Eppendorf) Epos selective analyser 5060 (Eppendorf) - Page 12 - 000487 11/09 '98 18:29 FA* 31706418543 NOTO* B.V. 015/017 l_ ______________________________________________ ___ ___________________________________ _ 1 TELOMER ALCOHOL/TELOMER ACRYIATEI /PFHS/PFOS NOTOX Project 242933 URINALYSIS (Recovery group animals only) 1 Urine samples will be collected overnight (approximately 16 hrs) from all animals assigned to the Recovery groups according to the following schedule: - predose 1 - during the treatment period on days 7, 14 and at the end of treatment - at the end of the recovery period, prior to scheduled necropsy. During the sampling period animals will be deprived of food but water will be provided. Urine will be collected Into a specimen vial, using a metabolism cage. After collection the samples will be frozen and stored at -20*C at NOTOX until further analysis. PATHOLOGY NECROPSY All animals surviving to the end of the observation period and all moribund animals will be deeply anaesthetised using ether vapour and subsequently exsanguinated. All animals will be necropsled and descriptions of all macroscopic abnormalities will be recorded. Prior to exsangulnation a blood sample (1*2 ml) for serum collection will be taken from the aorta. Serum samples will be stored at -20*C at NOTOX until further analysis. J Samples of the following tissues and organs will be collected from all! animals at necropsy and fixed 1n neutral phosphate buffered 4% formaldehyde solution: Identification marks Adrenal glands Aorta Brain Caecum Colon ] Duodenum Epididymides Eyes with optic nerve and Harder1an gland Female mammary gland area Heart Ileum Jejunum Kidneys Liver Lung, infused with formalin Lvmph nodes - mandibular, mesenteric Oesophagus Ovaries Pancreas - Page 13 000488 11/09 '98 18:30 FAX 31736418343 NOTOX B.V. Ql 018/017 THIOMER ALCOHOl/TELOMER ACRYLATE/ /PFHS/PFOS NOTOX Project 242933 Peyer's patches (jejunum, Ileum) 1f detectable Pituitary gland Prostate gland Rectum Salivary glands - mandibular Sciatic nerve Seminal vesicles Spinal cord -cervical, mldthoradc, lumbar Spleen Sternum with bone marrow Stomach Testes Thvmus Thyroid Including parathyroid. Trachea Urinary bladder Uterus. All gross lesions ORGAN WEIGHTS | The following organ weights (and terminal body weight) will be recorded from the | surviving animals on the scheduled day of necropsy: Adrenal glands { Brain j Heart 1 Kidneys Liver 1 Ovaries I Spleen J Testes $ ] Both absolute and relative (% body weight) organ weight data will be Included 1n 1 the study report. ."x 1 LIVER SAMPLING * From all animals surviving until the scheduled necropsy at least 1 gram of the left lateral U v e r lobe will be frozen 1n 1sopentane/N2 . Liver samples will be I stored at -20*C at NOTOX until further analysis. I i - Page 14 - 000489 11/09 '98 18:30 FAX 31738418543 N0T0X B.V. 017/017 l--------------------------------- -- - _________________ ; 1 i TELOMER AlCOHOL/TELOMER ACRYLATE/ /PFHS/PFOS NOTOX Project 242933 HISTOTECHNOIOGY All organ and tissue samples, as defined under Hlstopathology (following), will be processed, embedded and cut at a thickness of 2-4 micrometers and stained with haematoxylin and eosln. Special stains will be used at the discretion of the pathologist. I HISTOPATHOLOGY v Slides of all underlined organs and tissues (see under Necropsy) collected at the scheduled sacrifice from all animals, as well as from all animals of all dose groups which died spontaneously or were terminated in extremis, and all gross lesions of all animals (all dose groups) will be examined by a 1 pathologist. All abnormalities will be described and Included 1n the report. STATISTICAL ANALYSIS The following statistical methods will be used to analyse the data: If the variables can be assumed to follow a normal distribution, the Dunnetttest (many-to-one t-test) based on a pooled variance estimate will be applied for the comparison of the treated groups and the control groups for each sex. The Steel-test (many-to-one rank test) will be applied instead of the Dunnetttest 1f the data can not be assumed to follow a normal distribution. All tests will be two-sided and 1n all cases p < 0.05 will be accepted as the lowest level of significance. Additional methods of statistical analysis may be used at the discretion of the Study Director. The methods and the results will be described in the report. References: I - C.W. Dunnett A Multiple Comparison Procedure for Comparing Several Treatments with a Control, J. Amer. Stat. Assoc. 50, 1096-1121 (1955). i J - R.G. Miller Simultaneous Statistical Inference, Springer Verlag, New York (1981). fi 000490 - Page 15 - TELOMER AlCOHOl/TELOMER ACRYLATE/ 7PFHS/PF0S NOTOX Project 242933 DISTRIBUTION This protocol will be distributed as follows: Original: 1 Copy: 1 Copy: 1 Copy: 1 Copy: 1 Copy: 1 Copy: Study Director Coordinating Bioteclmldan Clinical Pathology Necropsy/H1stotechn1que Hlstopathology Management Sponsor .X f 000491 STF HIS 325/03 H^NOTOX Safety& EnvironmentalResearchB.V. SPECIMEN DISPATCH LIST NOTOX PROJECT: 242933______ SPECIES: RAT TEST SUBSTANCE: 83484, 83494, 83502, 84456, 84141 SIGNATURE/DATE STUDY DIRECTOR: ShUrCQ-- - 1Q39 TO: Name and adress company: 3 M Environmental Technology and Safety Services Attn. Kris Hansen 935 Bush Avenue Building 2-3E-09 SsA ^ 'S f f S l ' j g l tel. 001 .6 s i T 32>5, CnnaruinT. Cca.se)_og oov L s C P o - u - L Lexter) 55 Group 1 Group 2 Group 3 Group 4 Group 5 Group 6 Animal numbers males 1-11 + 13-15 17-27 + 33-43 + 49-59 + 65-75 + 81-91 + 29-31 45-47 61-63 77-79 93-95 Animal numbers females 97-107 + 113-123+ 129-139+ 145-155+ 161-171+ 177-187 + 109-111 125-127 141-143 157-159 173-175 189-191 Number of U v e r samples 28 28 28 28 28 j. 28 Also enclosed are : [ ] Copy of Protocol/Amendments [ ] Copies of histology raw data [ ] Study results [ ] Necropsy data transfer file [] DISPATCH: Signature: Date:. 0 I7.i2f0>.... PLEASE SIGN AND RETURN THIS FORM AS SOON AS POSSIBLE AFTER RECEIPT: COMPANY/SIGNATURE. C d & . A . ...?/*\ Date:... D ^ J . O? /. ^... CC0492 ^ Lisa A. Clemen 02/06/99 04:20 PM Environmental Technology & Safety Seivlcea (651)778-5568 3M Building 02-3E-09 PO Box 3331 SL Paul, MN 55133-3331 Fax: (651)778-6176 To: Kris J. Hansen/US-Corporate/3M/US@3M-Corporate Kail J . Rambo/US-Corporate/3M/US@3M-Corporats G rant A. Paul/US-Corporate/3M/US@3M-Coiporate cc Subject: NOTQX 242933 Sam ple Receipt On 02/03/99 we received 168 rat livers from NOTOX 242933 (TOX120, W1220). These samples were received frozen on dry ice and have been stored in Freezer 9 at -20 +V10C. Lisa SAKPUE3 tJjEQjuffc 4 V B R i F i e b 000493 3H Environmental Technology and Safety Services attn. Kris Hansen 935 Bush Avenue Building 2-3E-09 St. Paul, MN 55133-3331 USA U M otox SafetyftEnvlronmantalResearchB.V. Hambakenwetering3 P.O. Box3476 5203OL *s-Hertogenbosch TheNetherlands Tel.: (073)6419575 Fax:(073)6418543 Date : 29-JAN-99 Ref. ; KIM Subject: NOTOX Test Substance No. 83484, 83494, 83502, 84456, 84141 Dear Kris, On request of Mrs. S. de Hoog herewith I send the liver samples (total 168) from NOTOX project 242933. With kind regards, NOTOX B.V. Mariette de Kinkeider Test Substance Officer enclosure: a.m. Liver samples 000494 Chamberof Commerce VHertogenboschnr. 16055281 NOTOX Project #242933 P e b .4 ,1 9 9 9 The liver sample numbers listed below did not include a collection date on their containers. After reading the protocol, I wrote the collection date on each container. See below for dates. If these collection are not correct, please call me at 1-165*778*5368. Regards, Lisa A. Clemen Ac Samples 1 2 3 4 17 18 19 20 33 34 35 36 49 50 51 52 65 66 67 68 81 82 83 84 Group 1 1 1 1 2 2 2 2 3 3 3 3 4 4 4 4 5 5 5 5 6 6 6 6 Collection Date Added 7 11/03/98 711/03/98 711/03/98 711/03/98 711/03/98 711/03/98 711/03/98 711/03/98 711/03/98 711/03/98 7 11/03/98 711/03/98 711/03/98 711/03/98 711/03/98 7 11/03/98 7 11/03/98 711/03/98 711/03/98 ? 11/03/98 711/03/98 711/03/98 711/03/98 711/03/98 Samples 109 110 111 125 126 127 141 142 143 157 158 159 173 174 175 189 190 191 Group 1 1 1 2 2 2 3 3 3 4 4 4 5 5 5 6 6 6 Collection Date Added 7 12/04/98 7 12/04/98 7 12/04/98 7 12/04/98 7 12/04/98 7 12/04/98 7 12/04/98 7 12/04/98 ? 12/04/98 7 12/04/98 ' 7 12/04/98 7 12/04/98 7 12/04/98 7 12/04/98 7 12/04/98 7 12/04/98 7 12/04/98 7 12/04/98 000495 NOTOX #242933 TOX120 Liver Samples Received 02/03/99 Samples -2 '3 -4 -5 *6 -7 '8 -9 '10 Nil >13 "14 <5 <7 -48 -19 "20 -21 "22 "23 "24 -25 . "26 <27 "29 "30 -31 "33 -34 "35 -3 6 *37 "38 -3 9 -4 0 Ml "42 '4 3 *.45 "46 "47 "49 -5 0 -51 -52 <53 N54 -55 "56 -57 *58 ^9 "61 -62 -63 Group 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 2 2 2 2 2 2 2 2 2 2 2 2 2 .3 3 3 3 3 3 3 3 3 3 3 3 3 3 4 4 4 4 4 4 4 4 4 4 4 4 4 4 Collection Date 11/03/98 11/03/98 11/03/98 11/03/98 11/04/98 11/04/98 11/04/98 11/04/98 11/18/98 11/18/98 11/18/98 12/02/98 12/02/98 12/02/98 11/03/98 11/03/98 11/03/98 11/03/98 11/04/98 11/04/98 11/04/98 11/04/98 11/18/98 11A8/98 11/18/98 12/02/98 12/02/98 12/02/98 11/03/98 11/03/98 11/03/98 11/03/98 11/04/98 11/04/98 11/04/98 11/04/98 11/18/98 11/18/98 11/18/98 12/02/98 12/02/98 12/02/98 11/03/98 11/03/98 11/03/98 11/03/98 11/04/98 11/04/98 11/04/98 11/04/98 11/18/98 11/18/98 11/18/98 12/02/98 12/02/98 12/02/98 Samples Group Collection Date --65 5 11/03/98 >.66 5 11/03/98 "67 5 11/03/98 -68 5 11/03/98 "69 5 11/04/98 -70 5 11/04/98 "71 > 5 11/04/98 <72 5 11/04/98 "73 5 11/18/98 -74 5 11A8/98 *75 5 11/18/98 -77 5 12/02/98 *78 5 . 12/02/98 "79 5 12/02/98 '81 6 11/03/98 ''82 . 6 11/03/98 -83 6 11/03/98 - 8 4 6 11/03/98 -85 6 11/04/98 <86 6 11/04/98 -87. 6 11/04/98 -88 6 11/04/98 "89 6 11/18/98 -90 6 11/18/98 -91 6 11/18/98 "93 6 -94 6 12/02/98 12/02/98 -95 6 12/02/98 -97 1 11/05/98 -98 1 11/05/98 -99 1 11/05/98 -100 1 11/05/98 J01 1 11/06/98 -102 1 11/06/98 "103 1 11/06/98 <04 1 11/06/98 -105 1 11/20/98 -J0 6 1 11/20/98 "107 1 11/20/98 "109 1 12/04/98 -110 1 12/04/98 -111 1 12/04/98 <113 2 11/05/98 <14 2 11/05/98 *415 2 11/05/98 <16 2 11/05/98 -117 2 11/06/98 ' <118 2 11/06/98 <19 2 11/06/98 "120 2 11/06/98 "121 2 11/20/98 -122 2 11/20/98 -123 2 11/20/98 -125 2 12/04/98 "126 2 12/04/98 -127 2 12/04/98 Samples \1 2 9 <130 -131 Group 3 3 3 Collection Date 11/05/98 11/05/98 11/05/98 <32 -133 -134 3 3 3 11/05/98 11/06/98 11/06/98 "135 3 <36 3 11/06/98 11/06/98 -137 3 11/20/98 "138 <39 3 3 11/20/98 11/20/98 <41 3 12/04/98 < 4 2 3 12/04/98 <43 3 12/04/98 -145 4 11/05/98 -146 4 11/05/98 -147 4 11/05/98 -148 4 11/05/98 < 4 9 4 11/06/98 < 50 4 11/06/98 "451 4 11/06/98 -152 4 11/06/98 "153 4 11/20/98 <54 4 11/20/98 \1 5 5 4 11/20/98 <57 4 12/04/98 <58 4 12/04/98 -159 4 12/04/98 <61 5 11/05/98 '-162 5 11/05/98 <63 5 11/05/98 -164 5 11/05/98 -165 5 11/06/98 "166 5 il/0 6 /9 8 -167 5 11/06/98 -168 5 11/06/98 -169 5 11/20/98 -170 5 11/20/98 <71 5 11/20/98 ""173 5 12/04/98 <74 5 12/04/98 <75 5 12/04/98 -177 6 11/05/98 >178 6 11/05/98 -179 6 11/05/98 -180 6 11/05/98 -181 6 11/06/98 -182 6 11/06/98 -183 6 11/06/98 N184 6 11/06/98 -385 6 11/20/98 . "186 -187 6 6 11/20/98 11/20/98 <89 6 12/04/98 -190 6 12/04/98 <91 6 12/04/98 000496 000497 *% ; IX / iiraM^TTTyjff<B,Wnir5tfg r , I. From (Collection Address) Sendbig Depot Receiving Depot ::0 iSander'sAccount No. i |0|1|6|0|9|5| 2 1 ` F'i w NOTOX SAFETY & ENVIRONMENTAL m *c RESEARCH BV HAMBAKENWETERING 3 * -s.. ^ GD840494663WW , a* 'S HERTOGENBOSCH iw/zipo*: f Proving: "** Country: 5231 DD NL **'' -v'X .C on act Name f " . V J X JL L Tel No: 0 7 3 6 4 1 9 5 7 5 m 2. To (Receiver) (If a different delivery address is required please complete Section A) U r i S M & kl& C ! < ? } If'.Addre 3 ^ r\0\<TVV\l<\fc,tXl "T C C-Uf) .&< jCaW M f- e,ojiCflS, ( X t f ^ cuje\AM.e. J i ovAA.tct-vvvn-"' 2l-"SE, ~ Oo Ccli r 1* ; I cWSt.ftwL* Postal/ZIpTodc f W l O Y S l $ 3 - 2 l Country: ^ Contact Nam y f ( yf\ . U o . w s g . , v ^ T iN ^ c)o .i^ n a ^ (x 3 t8 A. Delivery Address (If different from Receiver's address) y /'M i m * ' CIV Proving: Contact Nam Postal / Zip Cod Country: TeiNo: ? 3. Goods (If dutiable please complete Section B) LGeneral DycrlpUon Anh NlM m fc P WNMnUtn k ri No of . . .. PKkat w f * Dtmenrieei (I Check j m B. Dutiable Shiment_Dotails (Comnlcir when .mnlignbloi :i V ^o x l - u o t L U O u L C \ L q fro a box b o ^ fi : c W w a j! rO v .L jO l * r C(Y v>V - 6U m te e . 1 y JJ 't XX x . x ' 1 Xx i NaOFMCXMQir--- .................... -....... - - ^ . WEIGHT(LBS) 8AT . 4,, HAA ' ' > 004150004 5 . 0 ^ ; Sat No.-" 4 . Services * 0 :; _ Total' OPS ftd u |* t Vfarifr. VWfttt \felmo Vbfarrw WW^m Sj h m World Sendee*. | | Kur t (t amMhwy) Q GawmtM i [2 j Priori ORIGIN LON SHIPMENT NO. M15Q0QM 4150004961 %1 004150004 ! 004150004 *-v'*r%' ;..''<j( *'' L|I JII'7PN-weittOettbArmytdfv.re^Wif Invoke Q StfxMr' f~ l * * .* >*tm ni . j <Stn<fiiW*fcfwpfl^ry$mr*wctT*| | %1 %1 %1 Nn 2*alfe.i 'VS^w,_/_:_ Y r -ji* -- ---------- -- ltu T O )N S SUMMARY SHEET t Study: Tir /<g> "/Analyst: ^ L/JZ./?? C 8ohcptftNNumb:/t&M'<SlS9 / Matrix: Y ^ 'p d c , ^ 000498 Notts: /2T ^ / / & " ur /:L - 522=U^ + ^^2/ y ff&z+t/s/p' y 000499 ir-*?# -- -- -- Sludy-^Vie^ DafeMnalyst: JSt/tet? ample num ber or dtsctpiHon wr A 3. J__ _/3Sf?. ______ /3?r f / ^ T _ _____ dieutTons summary sheet AtSJ& J/YpZ& r* SobepOTN Number: /& b*' 7? w s& s? Matrix: Noies: /?* "f s&> % t I 000500 DILUTIONS SUMMARY SHEET Study: T * * / t o , , ,,, , Dilution Date/Analyst: s f a h q / A " ** Box#: '7% 3?& Solvent/TN Number: f f ' * A / t ~V -A -J.J # Extraction Date/Analyst: M atrix/T im epoint: Uve/' . sample number D IL U T IO N S o r deserpition 1: ) r v 1: w o v 1: 1: 1: 1: 1: 1: 1: Comments too. l i f - a j r X ___ (o ff- M b- lo s-p - toe,F~ >o?f- } 177F- & fttf- 1s ... ?C- ft f- Imp- tV -F - MPMP- tfS F - lUF,, II?P- n i9 /= 9fi=- =^i N otes: I ' . f O P O '11 l u J / - -- Ly I'/ m J /-serf t (OoOtJ r tfo ij- 1 * DILUTIONS SUMMARY SHEET Study: 'fb'Ar&fi Dilution Date/Analyst: QAc* i Box#: p-tiCfAtfi t __ .W Solvent/TN Number: MjU$ , 9 , Extraction Date/Analyst: Matrix/Timepoint:y P d ^ tr sam p le n u m b e r . o r deserpition O SA 65 aA C lA 1:5*00 t * I'.is o . v .a s 1: 1: ( j/ c< lA 7o A 7 /A i 13/ 1 3 /A 7y /i V,/ X 71/ j n .A 77/ 17/ 17/ i7 / v/ 63 / X % n/ oiopP ' a t/ 23/ \/ V/ Noles:^./ i ' S W - 3 'Q/jJ. & ~ t f A c 'V l ^ L f . z f O - V.O/J. S L -p lt : 796/ ^ l a Uj j H I.as' A Vty*L : 9 C,D/*l A c O H DILUTION S 1: 1: t i ' * I: 1: . fAH,-XP, o o o J Comments 000501 000502 DILUTIONS SUMMARY SHEET Study:~fo%ft2Q _ Dilution Date/Analyst: tC IIWJAP Box#: W-'VClftiG ' Solvent/TNNumber:Midi, JhrA'&OT Extraction Date/Analyst: /5Aprfffl, fM XPt J'fir* Matrix/Timepoint:AdUyjcT sam p le n u m b e r DILUTION S o r descrpition 1: 2 S 1: / 0 1: I: I: 1: 1: I: I: Comments ' -& /A X uH / ( - Z G aA ________ / - 3 3 A ____6 3 ___________ 3V /I 3 iW 3L/ 3 1 /A 3M 1 7 /1 HO/ ^/ %// y j A c,2 2 9 /1 3O A n /1 J X A m m <42/1 6 3 45/ w 1 1 H C / J/ V/ N otes: A f : Q f = H O ^ l f ^ k Mi l:fO - fOO^L f*yfk : JOQ/-L / O 0 v * . .. * DILUTIONS SUMMARY SHEET Study: -fbX-lQ.Q Dilution Date/Analyst: B ox#: 19-0(,IAtQ f7^ / 3 ^ Solvent/TN Number: /MK, -rU -A -W f Extraction Datc/Analyst: Apr UH,dtPt -pp Matrix/Timepoint: at Lvcr ' sam p le n u m b er D IL U T IO N S o r descrpition \ u o I: 1: I: I: 1: 1: I: I: Comments itfM 6 3 \ t 000503 . , * . / ! * Notes:: dL>( tto - W O ^ L r^yik, 1M/*L ft) % Study:Tox-iao Dilution Date/Analyst: * *' 9 9 - 0 (a A f> sam ple number or dtserpition 4M >3 HO b io DILUTIONS SUMMARY SHEET ^ Solvent/TN Number: MxH (T ru -ri -q s o (* Krtr^dk Drt^Aiudyst: W f-f^//z ji/w-jc/>-s u r - w y MWrhmmepoliit:p .^ u ^ DILUTIONS 0 1: 1: 1: 1: 1: 1: Comments S '3 7- ? ? S c*-' ------ - 000504 * . ' . / 0 *0 o ^ ------------------------ Notes: (Moto L ffi SOJrtfi* ^OO juL n u o ti * 0 DILUTIONS SUMMARY SHEET StadrTbX-120 . DihiUonDale/Analyst:"/<3/99".AH SExotlvreanctt/iToNnDNautme/bAenra.Mlys(t6:W)/i fJ ^ *-< r)- b n ____________________ __________________ Nfatrlimmepotoh /|VfK / ordescrpitionsa m p le n u m b e r D IL U T IO N S 1 0 0 0 I: 1: I: 1: I: I: 1: I: % l M t Gvlff D lO O fl j TIM . . H M . TKM S 1 Tl.M . nM . M , . M , Comments >IM . KM , Ihm, K .m ' L_______ \L _ .. r b r l T 5 c> * "4 m 0 Notes: DJOOO - ScmpU f IOOOmL wdbaml -------------v - - -- , /TCP 000S05 000506 DILUTIONS SUMMARY SHEET Study: iW rt^O Dilution Date/Analyst: PTM* g>0X 99-W A*t> Solvent/TN Number: ^ ^ W SS . Extraction Date/Analyst: y //? /? ? j IVSi/jCfi/SCr/SAf/ Matrix/TImepoint: f r f ^ / f r 0Ur f ____________ ordescrpitionsam ple n u m b er DILUTION S I: 7 0 1: 1: 1: 1: 1: 1: 1: 1: Comments WM 6H 0/4 SOM W 1 StM M O M iV SiM S-tf SUM M - mw V/ * : ` / % % * Notes: Oio- oomL sw p U t I mL /m ^ W % v Sample weights/Volumes Prep Date(s): Analyses): f l 3 C )9-~ Sample Matrix: Pli r L-i u * * Method/Revision: /-'/T c 7"'/'! -f> O Target Analyte(s): / Study Number *T~0 K ( P - 0 Equipment Number: Notebook# and Page: Final Solvent/TN Number 1MG1 2MG1 3MG1 4M Gl ] 3MG1 6MG1 7MG1 1 8MG1 9MG1 OMGI UM Gl 13M Gl 14M Gl 15MG1 17MG2 18MG2 19MG2 20MG2 21MG2 22MG2 J 23MG2 24MG2 25MG2 26MG2 27M G2 Sampie ID Initial Wt/VoL g/mL/L ,6 s i ?r /0,/g f ? 9 >,5/2~ A.&91L0 /9*. A). 9a.S 0. 3W #ml MQ Water Added 33 3 . S" `C> 3M V-S /. 1 ... 3.2, 2.S V-3 / . 7 / SM M /W 4 M S // H.S V.3 A 503 S3 > -9 9 ? 3 S.o 33 ^5^3'/ 2 .1 Pf (2, h S 7 ? - ' 9 .0 A 3 & F ir 0 72VT 03910 S3 3.6 3.0 o stri ti7 3 * i 0.9/7^ 7. 7 9iC Density(g/ml) .\ Comments ' ^-- > * *"! . J /^(i Alf J ffL fJ flrl1A i e j SU fjr by O h ( M i *~p }*f h /*,/& / USf u O /? 9 V *tf>l)r J jty f lg } / Notes: > a m K-y ^ s n /s r A ? J Extraction-1 Template Review Date______ _ Form Approved by/Date:_ \ Weight Volume Sheetl20.xls 000507 Page 1of_ Prep Date(s): Analyst(s): A jJltbJcP 'J'A P Sample Matrix: Method/Revision: fA -fT -'/l-ftQ 1 Target Anaiyte(s): Sample ID 29MG2 30MG2 31MG2 33MG3 ] 34MG3 35M G3 36M G3 37MG3 38MG3 39MG3 40MG3 41M G3 42MG3 43M G3 45MG3 46MG3 47MG3 49MG4 50MG4 51MG4 J 52MG4 53MG4 54MG4 55MG4 56MG4 Summary of method: ] Sample weights/Volumes Study Numben / O Y f j u p Equipment Numben Notebook# and Page: Final Solvent/TN Numben Initial Wt/VoL g/mUL #ml MQ Water Added Density(g/ml) 45/3 -Pfr / / />*SS S W .<&/*/ H * .V& 3 Z - O.GHS- 3.H .ra sa Sb/3. O e>- / . w a s 4.> 3 .0 as?-`/_ LA .iSbio Z .L 3/3~ a ) /. /53 J,73/3 3 .7 V.3T s: 3 ~y& ~ M ?// 3, i 3., A.V/5- 3 . 2 .sSit Z .S Z.l YO 25%? in q >.5-/9 3 -3 .. Comments Notes: <D Z ! 1 Extraction-1Template Review Date__________ Form Approved by/Date:. WeightVolume Sheetl20.xls 000508 Page 1of PrepDate(s): ] Analyses) : / # j A P Sample Matrix: Method/Revision: D Target Analyte(s): Sample ID 57MG4 58MG4 59MG4 61MG4 62MG4 63MG4 65MGJ 66MGS 67MG5 68MG5 69MG5 70MG5 71MG5 72MG5 73MG5 74MG5 75MG5 77MG5 78MG5 79M G5 81MG6 82MG6 83MG6 84MG6 83MG6 Summary of method: ] j Notes: 1 I Sam ple weights/Vohimes Study Number: *TPX / Q Equipment Number Notebook# and Page: Final Solvent/TN Number: Initial WL/Vol. g/mL/L n .m i d . q a i _ /. m i l ? t.o i /.a m o.xo& t d.1Y73 t.O & Y O .Q T 7 7 0 .1 9 o 3. &95/C, t.o u rc 1.027 0.99 o 0.9*130 o .ifo ? 1 .0 9 0 3 D .qw j 0 .-7 1 6 V 0 .9 7 0 3 0 .1 7 a S ' /.o il! #mlMQ Water Added .T H.C ?.v - ny f.y t/. x 2. / 0 -- sU y .9 </.Y -r.3 ! 3 . 3 f.O to 3. Jr y .i 1 .7 3 .9 **3 Demity(g/ml) Comments , .. Form Approved by/Date:. Extraction-1 Template Review Date________ Weight Volume Sheetl20.xls 000509 Page 1 of Prep Date(s): y A f f o 9 Analyses): Sample Matrix: / t x f / v y * Method/Revision: p ^ - r p - r f - f . Z> Target Analyte(s): Sample ID 86M G6 87MG6 88MG6 89MG6 ] 90MG6 91MG6 93MG6 1 94MG6 95MG6 Sample w e i g h t s olumes Study Number: "~p Equipment Number: Notebook# and Page: Final Solvent/TN Number Initial Wt/Vol. (dmUL C>'9Pt .Z37X M l Li 1>%sO i-o n L I.T33 , 9 ItOJ-Y 1-/037 ftnIMQ Water Added y* yz `t ' 9 s .9 SI3 S* J&v/ Y* S S7f S* S Density(g/ml) Commenta - A J *t 3 Notes: i ! J Extraction-1 Template Review Date________ Form Approved by/Date: Weight Volume Sheetl20.xls 000510 Page 1of. Extraction Worksheet ETS-8-4.0 Study # T / ? y >1.0 Surrogate Std Box #. 9 f ^ C 7 A / 6 MatrixJ U jU * J L - approx. ppm actual/#) ppm # AL *UQ 9 __ -A.6Kiit-H.l- __ _________ -LAZ/U-tL -SaJ - N I - -/Ajt.k--N )- FC -M ix approx. 0.5 ppm actual ppm ______ FC -M ix approx. 5 ppm actual ppm # 99t>// - / - ) - FC -M ix approx. 50 ppm actual ppm * 9 9 * //Y J l<J - Date and Initials for Std. or Comments fitti M-W*< ta.lM J 7 ^ .0 7 1 1 l1^ *L-M^ \M Cl pM Cl 0 Cl m Cf KM Cl Vt io J - - 10J. 7D - - .- I/ JCP-Si i LM ir! m rr fif Cl ?M iM IbM C l UM C l IM C l m Cl km a FfM C 2 m 6-1 --1 Vr -- - .- - - - , ^ * ' t 1Study num ber w here tihe originiil workshetf is located. ____;_______________:__ ____,-_ _ i-- L_-- , " ~ Blank / / , U J / . ^ a Std# - ? 01 1 - S^2t> am ount- ItO mL fa . 1 7 9 4 a L /S Serum Extraction Method : P < Date & Initials- Vortex 15 sec. Pioette Matrix Volume A ml Y/re/fQ ` Pipette 1ml of 0.5 M T B A pH 10. Std.# 9 9 H - Y - 2 . S A U l I Z I jUIjJ V / l if o ? Pipette 2 ml o f025 Na?COV0.25M NaHCCh buffer Std. # 9 9 a / U SS~A ' Dispense 5 ml of methyl-t-butyl ether TN-A- 2 X Shake 20 min. Centrifuge 20-25 min. Centrifuge speed: .A T ^i> Remove a 4 mL aliauot of oreanic laver Put on Nitrogen Evaporator to drvness Evaporator#:___________________Temperature:__________________ __ Add methanol Volume 1 .0 ml TN-A- aM Zfc Vortex 30 sec. Filter using a 3cc B-D svrinee with a 0.2um filter into a 1.5 ml autosamole vial > n o n v i o v t / p v*uiu. u i c t iu . o p iN c u t u uju u i a __ ' i_r_ / i ppm. MS/MSD used ssaample ) Cont. Checks used same m atrix as for std curve. SJuurrrroogate Standard: Spik'--ed1 J~ uL o f a S~~ ppm std f 9 9 a / / ) to all sam ples, standards, and blanks (j) fth-nxp I- <. J r t 6 ) } MS2.-t-tjpi.~j/nllc /JStf Attachment A ETS-8-4.0 Extraction of PFOS from Serum Page 10 o f 13 000511 Extraction Worksheet ETS-8-4.0 W OE !BOE Jit>TBF`lCW Surrogate Std B o x m - g u t M t approx. ppm Matrix J2s /VA r actualJOO PPm FC-Mix approx. 0.5 ppm actual ppm # AA f r i a m fri - ____C m L______ .- 1 M fri aaAf f r i - 3lM fr i - MM fri- S tM f r i - aiA t fr i ~ aw # fr i- fo/M f r i n m fri m fri U M fri ViM ( t i . S to iti VM ( t i 9 A fri 3tM fr i fri W M 64 VM fr i * ilM f r i ____________ - 1 Si TAI f r i iti V?M fri M P i sm M . %A ________ - ASudx .number where thie original workshSSit is located. Std# s i f w a m . Serum Extraction Method FC-Mix approx. 5 ppm actual ppm # - FC-Mix approx. 50 ppm actual ppm It - - Date and Initials for Std. or Comments 1 1 1 - _ . ,, amount ]_. O 1---------T - ____ i / mL^inQ^ e J k h Sii,1 Pate & Initials Vortex 15 sec. Pipette Matrix Pipette 1 ml o f 0.5 M TBA, pH 10. Volume Std.# Ac?- ml ?/(*/**s i O *. ~tr & mzmswmm Pipette 2 ml of 0.25 Na2CCh/0.2SM NaHCCh buffer Std. # 9 9 o /P -fT ^ Dispense 5 ml of mcthyl-t-butyl ether Shake 20 min. Centrifuge 20-25 min. Centrifuge speed: 3Sl)f) Spi*1 Remove a 4 mL aliquot of organic layer Put on Nitrogen Evaporator to drvncss Evaporator #: Temperature Add methanol Volume A O ml TN -A -SH M .& > t f j Vortex 30 sec. Filter using a 3cc B-D syringe with a 0.2um filter into a 1.5 ml autosample vial ________________________ MS/MSD/ I f Cont. Checks: Spiked 10 J tL o f a ppm std ( 'l for a final concentration o f C )r 3 0 ppm. MS/MSD used sampled?) UgI jTUJ ___ . Cont. Checks used same matrix as for std curve. Surrogate Standard: Spiked ( 0 uL o f a C ppm std ( ) to all samples, standards, and blanks 3M6-I f MSaM spS - spitt itMi-l, M -piti 13*6-1 A ttachm ent A E T S -8 -4 .0 Extraction o f PFOS from Serum P a g e 10 o f 13 000S12 Extraction Worksheet ETS-8-4.0 > i Study Box W M M B Matrix E r t f i W ST//M (rH SA V - obrj/M* ? cSM b# (Ur fi - AV- 6-V - ~~ Surrogate Std approx . ppm actual/ ppm # 9 fo /J I FC-Mix approx. 0.5 ppm actual ppm # - - FC -M ix approx. 5 ppm actual ppm # - FC -M ix approx. 50 ppm actual # ppm - - Date and Initials for Std. or Comments ' STA1 A f - 4/H A V - 1 /A M -- & M &*/ - M M tr*i - fcCAf A.C U M AT - - M M fri: - MM AC - MM a t \ \P WlAI A T AT - ^A 4 AT JIM AC - AT toW A C AC - - - ?fA f AC -- -- IF 7 K 7 K 7 9 H H H % L_______ - - - t~ 1Study num ber w here thie original w orksheet is located.----------------------------------------------------------------------------------:-- std# w a - c * a o amount = !,(j 1Serum Extraction Method Date & Initials Vortex 15 sec. Pioette Matrix - P.-- ~ ' Volume /. t? ml ------------- s:--- H Z Pipette 1 ml of 0.5 M TBA, pH 10. Std.# Pipette 2 ml o f 0.25 NaiCOV0.25M NaHCCh buffer Std. # _ /s~o w y** ^ Dispense 5 ml o f methyl-t-butyl ether TN-A- 2 JT<9 Shake 20 min. Centrifuee 20-25 min. Centrifuee sneed: 'idX)/tY\ / Remove a 4 mL aliauot of oreanic laver Put on Nitroeen Evaoorator to drvness Evaporator #: Add methanol Volume l*0 ml Temperature: TN-A- ZV3K 1Vortex 30 sec. 1. Filter usine a 3cc B-D svrinee with a 0.2um filter into a 1.5 ml autosamnle vial uL i _________________ 0 . 3 r d ppm. MS/MSD used s a m p l e _____________ Cont. Checks used same matrix as for std curve. Surrogate Standard: Spiked 1IU0 UuLL otf a ppm std ( 7 7 0 / / - // t o - / )) to all samples, standards, anud boliankxs <DMSjmpl-Sf'ilt 3M 6~lj AASa/MS0-5f))ce (jM fjt M3/MSP3 'S f i & A ttachm ent A E T S -8 -4 .0 Extraction o f PFOS from Serum 000513 Page 10 o f 13 Extraction Worksheet ETS-8-4.0 Study U T X -t Box A4-8 Matrix E A f /V<Y Surrogate Std approx, ppm actual/O ppm FC-Mix approx. 0.5 ppm actual ppm # FC-Mix approx. 5 ppm actual ppm FC-Mix approx. 50 ppm actual ppm # Date and initials for Std. or Comments iy/o -fe.-ftrft fr yfl_ n m &<r INLJrk.z. 66- 6L J *. '}M frit - Of $ H M 6r(r fm J i k . J f l 1 - rfiP, o nnT~i! r M&1 rH75 / J M M -- MS' TEL t JL MM (rio M l : or swvu / ^ g - L h j r f or/l, S A t t X 7l*>/79 - a h/f - AS V s 1study number where the original worksheet 5 tocatL Blank K flM irf F ivelT Std# m j p - W z Z T T amount8 Serum Extraction Method ,/ajr Zzfr.. Vortex 15 sec. Pipette Matrix Volume E E ml Pipcttc 1 ml of 0.5 M TBA, pH 10. Std.# */~2- jU L mL m n x i t i m t j k i t Date & Initials Pipette 2 ml of 0.25 Na?COV0.25M NaHCOt buffer Std. # h e / / --/ ? O Dispense 5 ml ofmcthyl-t-butyl ether Shake 20 min. Centrifuge 20-25 min. TN-A- jZ ? S Centrifuge speed: Z*Ul'ff Remove a 4 mL aliquot of organic layer Put on Nitrogen Evaporator to dryness Evaporator #: Add methanol Volume I*0 ml Temperature: TN-A- Vortex 30 sec. Filter using a 3cc B-D syringe with a 0.2um filter into a 1.5 ml autosample vial MS/MSD/ IK C ont Checks: Spiked 10 uL o f a S* ppm std ( ^/ ) for a final concentration o f _ ppm. MS/MSD used sampled?) h , f j /~Ia J Cont. Checks used same matrix as for std curve. Surrogate Standard: Spiked 1 0 uL o f a A ppm std ( % / / - / - , / ) to all samples, standards, and blanks M Sl/M S0/-spi& 3/l4fy rftejAASOJ-sfijce bM MS3/MSPJ - y l f a !3M l Attachment A ETS-8-4.0 Extraction o f PFOS from Serum 000514 Page 10 o f 13 IonPair StandardCurves--TOX-120(Rat Liver) PrepDate(s): Analyses): SampleMatrix: Metbod/Revblon: TargetAnalyte(s): 4/19m SAH/RWW/JCP/SRP RatLiver FACT-M-1.0 POAA, PFOS, ,PFHS, M513andM613 FC Mix StdApprox.0300ppm: FCMix StdApprox.5.00ppm: FCMix StdApprox.50.0ppm: SurrogateStdApprox. 100ppm: 99011-16-2 99011-16-1 99011-124 99012-3-24 . ActualConcentrationsofStandardsintheFC Mix POAA PFOS StdCone. ug/mL StdCone. ug/mL StdCone. ug/mL 0.500 0.500 0300 0300 0300 0.500 0.500 0.500 0.500 0.500 0300 0.500 0.500 0300 0300 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 50.0 50.0 50.0 PFHS StdCone. ug/mL 0.500 0300 0.500 0.500 0.500 5.00 5.00 5.00 50.0 CalculatedConcentrations ofStandards in theSampleMatrix. POAA PFOS Final Cone. Final Coric. Final Cone. ng/g ng/g ng/g 5.56 11.1 536 11.1 536 11.1 27.8 27.8 27.8 55.6 55.6 55.6 111 111 111 278 278 i 278 556 556 556 833 1111 833 1111 833 1111 PFHS Final Cone. ng/g 5.56 11.1 27.8 55.6 111 278 556 833 1111 StudyNumber TOX-120 EquipmentNumber Final SolventSt TNNumber MeOH/TN-A-2438 BlankTlssue/Identifler RabbitLiver/ 99012-5-20 M513 StdCone. ug/mL 0.500 0.500 0.500 0300 0.500 5.00 5.00 5.00 50.0 M613 StdCone. ug/mL 0.500 0300 0300 0300 0300 5.00 5.00 5.00 50.0 All AmtSpiked mL 0.002 0.004 0.010 0.020 0.040 0.010 0.020 0.030 0.004 All Density g 0.180 0.180 0.180 0.180 0.180 0.180 0.180 0.180 0.180 MS13 Final Cone. ng/g 5.56 11.1 27.8 55.6 111 278 . 556 833 1111 M613 Final Cone. ng/g 536 11.1 27.8 55.6 111 278 556 833 1111 Surrogate StdCone. ug/mL 100 ' Surrogate Final Cone. ng/g 2778 All Amt Spiked mL 0.005 Surrogate Final Cone. ng/mL 500 POAAJFOS,. ,PFHS.M513J4613.xls 000515 />?X 7?~37A*t Ion Pair Extraction Worksheet Study # T o* H-,0 Blank - { 4 -- /h iis t- t v e r Blank-/?. W L0 A 1 _______ - t n J - ______ - S S - 1 -7^ - Surrogate Std approx. ppm actual M t^ p p m #W ^ A tH U tf FC M ix Std approx. 0.5 ppm ' actual ppm #W 990//V S -L JsJ 0 * 4 _______ i_ FC M ix Std approx. 5 ppm actual ppm #W 990//-U -I * - 10J FC M ix Std approx. 50 ppm actual ppm #w 9 ? o //-/i< l Date and Initials for Std. or Comments w n a zn m \ -- V " m"f m ' I ~ 7SHa*k ~ 1______ - / t t e L i s l > / ~ 2s i.'i-sst.H t r f)f4. le s . M5 f)NO. llO p---l-lSdnA , HIS tL> I M w s' - .3 e J fod 7D. /s. / ( /ttiu ! . r f t '. o e S s~ -J~i *-i ts f r u /! > _____^ Shf >* _ -- 1-- ___ - -- ----- ' -- - ___ -- ^ ! i = = = = = ----------- = " ------- Blank B A I ,+L,u* r Std# ^ X 0 ? 9 -/S ^ 3 amount = Extraction Method Number/Revision:__________________________________]____________________;_____________ Date A Initial Add Surrogate, Vortex 15 see__________________________________________________________________ S JU + IK U M Pipette Sample Volume A t? mL Pipette 1 mL o f 0.5 M TBA, pH 10. Std. # G ? o 9 ^ S * r - /J Pipette 2 mL of 0.25 NaoCOV0.25MNaHCOt buffer Std. # 7 9 f ? -<? Pipette 5 mL of-ethyTacetate fa tJ - AhiJt4 TN-A- X Z S 7 Shake 20 min. Centrifuge 20-25 min. / Centrifuge speed: kJ 'O oc> Remove a 4 mL aiiauot o f organic laver Put on Nitrogen Evaporator to drvness Evaporator #: Add methanol Volume / , c) mL Temperature; / ( . SS-bJA_____________________ TN-A- 3?3Z S ' Vortex 30 sec. 1Filter using a 3cc B-D svrinae with a 0.2um SRI filter into a 1.5 mL autosample v i a } ______________________________ i t ____ -- M S/M SD/ f y ConL Checks: Spiked (0 u L o f a S ~ o o ^ std i f9 eJ )-S S -t ) for a final concentration o f 3J1? opl . M S/M SD used sample M o ^ r . Cont Checks used same matrix as for std curve. Additional Comments: 000516 f r y 7-43=tA*B r L _______ _______________ . IonPair StandardCurves-TOX-120 (RatLiver) Prep Date(s): Analyst(s): SampleMatrix: Method/Revision: Target Ana!yie(j); 2/22/99 RWW/SAH RatLiver FACT-M-1.0 POAA, PFOS, PFHS.M513&M613 StudyNumber: TOX-120 Equipment Number: Final Solvent& TNNumber MeOH/TN-A-232S BlankTbaue/Identilier RabbitLiver/98099-15-3 FC MixStdApprox.O.SOOppm: FC MixStdApprox. 5.00ppm: FC MixStdApprox. 50.0ppm: SurrogateStdApprox. 16.5ppm: 99011-16-2 99011-16-1 99011-124 98094-12-24 1 ] 1 I 1I Actual ConcentrationofStandardsintheFC Mix. POAA PFOS ' StdCone. ug/mL StdCone. ug/mL StdCone. ug/mL 0.500 0.500 0500 . 0.500 0.500 0.500 0.500 0.500 0500 0500 0500 0500 0.500 0500 0.500 5.00 5.00 5.00 5.00 5.00 5.00 5.00 50.0 5.00 50.0 5.00 50.0 PFHS StdCone. ug/mL 0500 0500 0.500 0.500 0500 5.00 5.00 5.00 50.0 M513 StdCone. ug/mL 0.500 0.500 0.500 0500 0.500 5.00 5.00 5.00 50.0 M613 StdCone. ug/mL 0.500 0.500 0.500 0500 0.500 5.00 5.00 5.00 50.0 CalculatedConcentrationsofStandardsin theSampleMatrix. POAA PFOS Final Cone. Final.Conc. Final Cone. ng/g ng/g ng/g 5.99 5.99 5.99 12.0 12.0 12.0 29.9 29.9 29.9 59.9 59.9 59.9 120 120 120 299 299 299 599 599 599 898 1198 898 1198 898 1198 PFHS Final Cone. ng/g 5.99 12.0 29.9 59.9 120 299 599 898 1198 M513 Final Cone. ng/g 5.99 12.0 29.9 59.9 120 299 599 898 1198 M613 Final Cone. ng/g 5.99 12.0 29.9 59.9 120 299 599 898 1198 J 1 ] 106F-G1 110F-G1 ms/msd 106F-G1 I10F-G1 POAA Final Cone. ng/g 299 299 InitialWt. (g): 0.9240 0.9242 PFOS Final Cone. . ng/g 299 299 Final Cone. ng/g 299 299 Initial VolumefmLV 4.6 4.6 PFHS Final Cone. ng/g 299 299 M513 Final Cone. ng/g 299 299 M613x Final Cone. ng/g 299 299 AU Amt Spiked mL 0.002 0.004 0.010 0.020 0.040 0.010 0.020 0.030 0.004 AU Density g 0.167 0.167 0.167 0.167 0.167 0.167 0.167 0.167 0.167 Surrogate StdCone. ug/mL 16.5 Surrogate Final Cone. ng/g 494 AU Amt Spiked mL 0.005 AmtSpikedfmLV 0.010 0.010 .J POAA.PFOS, .PFHS.M513.M613 000517 Sam ple W eights/ Volumes Prep Date(s): 1 Analyses): f a o I Sample Matrix: flifi-t 1 Method/Revislon: Target Analyt*(s): 1,0 Study Number. Equipment Number Notebook# and Page: Final Solvent: SfA f o . f Sample ID io.97P-D/ />m. 91 * 0 / / 0. /00 jP-- &-) r)N.a! t?~t f) Di. )oJ F--D} Initial <^yvoL /fonUL 0,nz 0 a </JJJ 0, J( . 0, w V 0, C.S70 ... . M 2 o,rifc. r 9X*/D DH. to? D-6-! >, </JJ~9 O//0> (>*7f 6~{ ' `/ / Z D Ain. h f - M aM . lIF- 6-1 6.92V2 0 .9H29 /Vim . \rtF-frli . ZO ntia. IMF-6-3 DA/i UPF- 6-3. h.W 9r b,0709 t.UOF-6-l ht 7-33ST DrJti, HI F`6-3 fan. l/t F-6-1 . 0.C3V .902 P/\Ja. 11$F-6-2 .P'm OaJsi. /OF -6-3 ,H29r Offa. 131F- 6-3 6.937-2 Cai*. 133 F -i-i_______________________ h. 039/ cU h & O j Comments l/hl ihr g m / m t a.(. 0.11,7 P . H - 6./OS' i . s ... 6 .1 7 2 3 .0 - ..St.^_____ p ?< r y-i. - ?s Htir j Q u l O O __________ 0.100. _ ./OH Ci.(00 h.ior n./Oc a.io? 2.0. ./aT .l /.O ./00__________ 0.11,7 Ht % JO A 6 . M 3. Z O - M 3.9 '0.100 3.0 ./0? 3 .3 .ior P U ./fer 2,1 0.100 PU 0.170 9.2 h, 100 3./ .M ] Summary of Method: Notes: J 1 Extraction-1Template 1 Review Date______ Fona Approved by/Date:. Weight Volume Sheebxls 000518 Page 1of Sam ple W eights/ Volum es Prep Date(s): P - ( i j ^ Analyst: f c M (S A H Sample M a t r i x : ^ / - Method/Revislon: pAfTZflA -J, Target Analyte(s): Study Number; YO )(*" / 2 Equipment Number: Notebook# and Page; F inalS olvent:^*///. ^ o M r Sample ID Initial ztSnpIVVoLL mL Meier Mn. MF-e-a .M aIa. i?rF-6-X o.su?v V0- ' Al. . W 3 .9 i Alp./ai-F- . 3t,0_ 3. / ' 0Ak./3F-<r .3CI2 - ONn. M F - <j O.'ttZ oma. .'rff m*. lilt-6-3 0.32/! _ A ? JDa}A.IFP- &3 a 0/3/ .. ?,/ ,Mfl. /ITT-3 o.rs/,9 ? Dftlfi.l2UF~6-3 2.9 J 0AlA.il??-i . m n V. jDAi/i.l2F~6r3 .(,*3$r _ 2J Aifi.ttfF-frl OaJ/. W P ^ I ..c o f o . 2.2 .003 3.3 ] PAJn.mF-Fi o,?*r? V,0 _ J 0A)n.W?f-6* 3* 7 DM, &.JH1 /,? jOn /).Ht-6-4 JH/t3 5./ J N. iw/e-frJ O,WS*? , f)N/>. HX/T-fr</ H/,99 5.3 j D/S. tWf-r ,&0?7 3,0 J f)rfO`iSoF-Ty_ _ _ _ _ _ _ _ rOVtC - 1 x 2 -- junoty Comments 3/#>C OJle? O.llp? .&? ___ o-iWt_ _ _ 0-n.f0-I/.SJU r>Jb?_ _ _ JS" DM O.ti? 0.1(*2 to'ib'i__ n.H.'* o.li.9 .Mrb O/bb OJFY 6.M fiJUt 6.m h.m (Ut. ? J Summary of Method: Notes: J , Extraction-1Template Review Date______ Form Approvedby/Date:. Weight Volume Sheetxls 000S19 Page 1of Sam ple W eights/ Volum es Prep D ate! z / t i f a Study Number: / / - / 2 - A Equipment Number Sample M a tite Method/Rerlsioa: / 6 Notebook# and Page: Final Solvent / ,/ Target naiyte(s): SaImDple $VIni/tViaolL dbM'ty Comments AfmLJL k/aU r W lrtL nrfo frfA - -tf - 51-P--AH n^,o. /r?/? -s</ n/ta,/JV /Z-9 A. ryy 'C t .Z s? $ >, 72.2. f t'Z o l 2 .7 3.2 9. 3,0 9.0 _CU(,1 ./r .M/& __ J 1 * 2 _n./6>? ntj. t r z P - o Y hrta. r s v f - a 9 o.ZfF l Z ,rys0 _r<n?<~ 9. 79 ,0 _6 M ' nfo? o -m //\f)M, U / f - a -r f)7/ 1 A ,fX f9 0 . * j9 9.9 3 .9 o -n . z 0 ,/u i f)NA. / / A-3~ 6 ,1 /0 ? 9J o ./i^ r /)///>. { s '/ '' o s ' 6,1/779 `*?it9 3.?2 .9 6.l(pb o .iu r o ,y irz 2.1 DH0. (6 7F - O S ' .< m z 2 .9 rOHt ((.7/C~-S' (7fi/ f - '/ S r f Tj<H 32 2.7- ./t- . D M , !7a F - A S ' . ??r? 3 1 .Kfi f7f F - A S ' /?Ha>. S' J[)/Ja , n i r - ~ A r ,r c ? i '7 7 t 6,1937 2? 9.9 9.0 ./M 0. Msb .lbfo Dno, A<r p,</z,z 2.5 n ./i T \ t/. n i/P - t- r . ___ _^0f9. f 7 f JSummary ofMethod: 6,7 TTZ 3 1 'YYZ-2-,. - A ,2 _, .M MT- 1. Notes: Extraction-1 Template Review Date______ I Fono Approvedby/Date:. Weight Volume Sheetxls 000520 Page 1of. Sam ple W eights/ Volumes Prep Date(s): Analyses): / l n / d / T A t f Sample Matrix: A tf-i-t* Method/Rerision: f A - r T - r t " / Target nalyte(3): Sample m ftl/a . 79 P o m . tDf-e-c. Paio, tfi P - & * j P/tJ, fXLf - S 6 nsia. 'n i ~/ZA nun. -c ] Oa/. lfV- ~/^a Pt/r j n f - A t fido. m f~- // Dlt, (?<)- r Pa/*}, [ `( o f - - ftNs*- A"-- C Study Number: *!~f/t - ( 2 - 0 Equipment Number: Notebook# and Page: . Final Solvent: 17, it* $ V*. Initial <WVol. t/mUL ft^-i JU&Ct'fc? pw/mL Comments .r/J~ JL*7 0 ,7 /* \V` I- *f.7 Y . J'C .X9V0 J* n./(*r .ii*s-____ ./bJ- ./or /)>2T/20,3/-0'7 .0*70 *3 YJ s:3 /*i- o./^r -.J U .L I ____ O ,!(o? .lbb O*/bip ... <j.Y .-Q.dlib:___ rCTf) j . Y M t*t 0*9(7 d Y' - ./L> J Summary of Method: ] I * (isti)* Extraction*1Template Review Date______ .y o**ft'Jf FormApproved by/Date:. Weight Volume Sheetxls 000521 Page 1of SOUP 020199: FACT Equipm ent Log 99014 Quattro II, #6414E PAGE DATE: 2/23/99 ANALYST: drb STUDY NUMBER:Tox-120 MATRIX: Rat Liver DESCRIPTION: Liver Samples FACT Method: FACT-M-4.0 . Injection volume: 10 uL Cycle time: 13.5 min. Mobile Phase: (A12.0 mM NH4CH3CQ2 Electrode: Z-Sprav (B).MsQH______ TN-A- or stndrd number (A) 98012-1-4__________ Prepared (date/by): (A12/11/99 hoi________ Expires: fAl 8/99 _________ O ) TN-A-226Q.__ (B1 2/99. hoi_____ (B )_ 8 /9 ________ Store at room temp? @ or N Other:___ G u ard column: None _______________ Part number: na_________ Lot number: na A nalytical column: Keystone Betasil_______ _____________________________ Size: 2 x 100 mm________ - ' . Type:_C18____________ Sphere size: 5 urn----------- Part number: 105-701-2__________ Lot number: P8C09 Serial number: 10881106D Analytical parameters: Drying gas fL/hrl: 300 ESI nebulizing gas (L/hrl 15 LC Flow rate: 300 nTAnin- Backpressure: 120 bar Sheath gas (L/hr)_Q____ EOPLC solvent gradient: Long 2 Time (min.) 110.00_____________ 21 8.50_____________ 3H L Q ___________ 41 12.0 51 13.5_____________ %B_ 40.0 90.0 M Q. 40.0 Stop 000522 Tuning Method Report Method Cs \MASSLYNX\FACT-1.PRO\ACQUBB\PFOS Printed: Tue Feb 23 15:59:26 1999 . ....................................................................................................... ______________ 5P U|> 0 2 Q L W Ot fe / /T ? IAC osftolti Page 1 BESTcopy AVAILABLE SOURCE ( ESP- ) CapillaryCone Extractor RF Lens Source Block Temp. Desolvation Temp. Set Rdbk 3.00 60 5 0.2 150 250 2.99 -60 -6 142 250 Pressures Analyser Vacuum Gas Cell Rdbk 7.8e-6 FAIL MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion EnergyIon Energy Ramp Lens 8 Lens 9 Multiplier Set Rdbk 14.0 14.0 2.0 . 0.0 55 650 Set Rdbk 15.0 15.0 45 2.0 0.0 40 0 650 42 39 44 000523 Scanning Method Report Method t C t\MXSSLmX\PACT-l. P*OUCQBDS\TOX120A Laet Modified: Tue reto 23 15:52x20 1595 Tinted: Tue feto 23 16:00:42 1999 Souq fta o M Solvent Delay < nina ) i 0.00 Function i 1 KMC of 3 Maas Pairs ( BSP- ) Inter Channel Delay ( S ec s ) : Span ( Daltons ) : Start Tins ( Mina ) : End Tine ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 13.50 1 Dwell (Sees) Coll Energy (eV) Cons ( V 1 399.00 80.00 0.25 2 399.00 99.00 0.25 3 399.00 130.00 0.25 45 45 45 60 60 60 Function : 2 MRM of 3 Maas pairs ( BSP- ) Inter Channel Delay ( Seca ) : Span ( Daltona ) : Start Tine ( Mina ) t End Tine ( Mina ) : Repeats i Channel Parent Daughter 0.03 0.00 0.00 13.50 1 Dwell . (Seca) Coll Bnergy (eV) 1 499.00 80.00 0.25 2 499.00 99.00 0.25 3 499.00 130.00 0.25 45 45 45 Cone { V ) 60 60 60 Function i 2 M M of 2 Maca eira ( SS- ) Inter Channel Delay ( Secs ) : Span ( Daltona ) : Start Tine ( Kina } : End Tine ( Kina ) Repeats : Channel Parent Daughter 0.03 0.00 0.00 13.50 1 Dwell (Secs) Coll Energy (eV) Cone V } 1 299.00 80.00 ' 0.25 2 299.00 99.00 0.25 45 45 35 35 Function : 4 ME M of 2 M u a aire ( BS- > Inter Channel Delay ( Seca ) : Span ( Deltona ) : Start Tine ( Mina ) : Bad Tine ( Mina ) i Repeats : Channel Parent Daughter 0.03 0.00 0.00 113.50 Dwell (Sees) Coll Xnergy ieV) Cerne ( V ) 1 2 3 413.00 119.00 413.00 169.00 413.00 219,00 0.25 0.25 0.25 30 20 30 IS 15 15 Function : 5 KMC of 3 Maas Pairs ( BSP- 1 Inter Channel Delay ( Sees ) : Span ( Daltons ) * Start Tine ( Mina ) : End Tine ( Kina ) < Repeats t Channel Parent Daughter 0.03 0.00 0.00 13.50 1 Dwell (Seca) Coll Energy (eV) Cone ( V ) 1 469.00 169.00 0.25 45 2 469.00 219.00 0.25 45 3 469.00 119.00 0*25 45 ,1 3300 30 Function : < KMC of 3 Mass Fairs { SSF- ) Inter Channel Delay ( Secs ) : Span ( Daltons ) i Start Tine ( Mina ) i End Tine ( Mina ) : Repeats t Channel parent Daughter 0.03 0.00 0.00 13.50 1 Dwell (Sm s ) Coll Bnergy l.V) Cone ( V ) 1 569.00 169.00 0.25 2 569.00 219.00 0.25 3 . 569.00 119.00 0.25 45 45 45 35 35 35 unction t 7 MBM of 1 Maas Pair ( a*- ) Inter Channel Delay ( Seca ) : Span ( Daltona ) : Start Tine ( Kins } : End Tine ( Mins : Repeats : Channel Parent Daughter 0.03 0.00 0.00 13.50 1 Dwell (Sac.) Coll Energy (V) Cone ( V ) 1 427.00 80.00 0.25 40 60 ib lAL-dlolll Page 1 . 000S24 M asslynx - Sam ple List 020Sample List: C:\MASSLYNX\FACT-1 .PRO\Sam pleDB\022399c.SPL Printed: Tue Feb 23 16:25:20 1999 r, 1#w. . DU ________________________________ S n u j> m LAC , S /t o m > Page 1 R ie Nam e File Text MS File In le t I Botti olum e Sam ple T j C one A C o n cB 1 022399020 MeOH Blank TOX12C long2 91 10 Analyte 2 022399021 MeOH Blank TOX12C long2 91 10 Analyte 3 022399022 Tox 120, RBL02229-H2O Blk-1,2 /2 2 TOX12C long2 1 10 Analyte 4 022399023 Tox 120, RBL02229-RBUVerBlk-1, 2 TOX12C long2 2 10 Analyte 5 022399024 Tox 120, RBL02229-5ppb-1,2/22/99 TOX12C long2 3 10 Standard 6 022399025 Tox 120, RBL02229-1 Oppb-1,2 /2 2 /9 TOX12C long2 4 10 Standard 7 022399026 Tox 120, RBL02229-25ppb-1,2/22/9 TOX12C long2 5 10 Standard 8 022399027 Tox 120, RBL02229-50ppb-1,2/22/9 TOX12C long2 6 10 Standard 9 022399028 Tox 120, RBL02229-100ppb-1,2 /2 2 / TOX12C long2 7 10 Standard 10 022399029 Tox 120, RBL02229-250ppb-1,2/22/ TOX12C long2 8 ' 10 Standard 11 022399030 Tox 120, RBL02229-500ppb-1,2 /22/ TOX12C long2 9 10 Standard 12 022399031 Tox 120, RBL02229-750ppb-1,2 /2 2 / TOX12C long2 10 10 Standard 13 022399032 Tox 120, RBL02229-1000ppb-1, 2 /2 TOX12C long2 11 10 Standard 14 022399033 MeOH Blank TOX12C long2 92 10 Analyte 15 022399034 Tox 120 DNO, 9 7F -G 1,2/22/99 TOX12C long2 12 10 Analyte . 16 022399035 Tox 120 DNO. 98F -G 1,2/22/99 TOX12C long2 13 10 Analyte 17 022399036 Tox 120 DNO. 99F -G 1,2/22/99 TOX12C long2 14 10 Analyte 18 022399037 Tox 120 DNO. 100F -G 1,2/22/99 TOX12C long2 15 10 Analyte 19 022399Q38 Tox 120 DNO. 101F -G 1 ,2/22/99 TOX12C long2 16 10 Analyte 20 022399039 Tox 120, RBL02229-250ppb-CC1, 2/ TOX12C long2 17 10 QC 21 022399040 MeOH Blank TOX12C long2 92 10 Analyte 22 022399041 Tox 120 DNO. 102F-G1, 2/22/99 TOX12C long2 18 10 Analyte 23 022399042 Tox 120 DNO. 103F-G1,2 /2 2 /9 9 TOX12C long2 19 10 Analyte 24 022399043 Tox 120 DNO. 104F-G1,2 /2 2 /9 9 TOX12C long2 20 10 Analyte 25 022399044 Tox 120 DNO. 105F-G1, 2/22/99 TOX12C long2 21 10 Analyte 26 022399045 Tox 120 DNO. 106F-G1, 2/22/99 TOX12C long2 22 10 Analyte 27 022399046 Tox 120, RBL02229-250ppb-CC2, 2/ TOX12C long2 23 10 QC 28 022399047 MeOH Blank TOX12C long2 92 10 Analyte 29 022399048 Tox 120 DNO. 107F-G1, 2/22/99 TOX12C long2 24 10 Analyte 30 022399049 Tox 120 DNO. 109F-G1, 2/22/99 TOX12C long2 25 10 Analyte 31 022399050 Tox 120 DNO. 110F -G 1,2/22/99 TOX12C long2 27 10 Analyte 32 022399051 Tox 120 DNO. 111F-G1, 2/22/99 TOX12C long2 28 10 Analyte 33 022399052 Tox 120, RBL02229-250ppb*CC3, 21 TOX12C long2 29 10 QC 34 022399053 MeOH Blank TOX12C long2 93 10 Analyte 35 022399054 Tox 120 DNO. 113F -G 2,2/22/99 TOX12C long2 30 10 Analyte 36 022399055 Tox 120 DNO. 114F -G 2,2/22/99 TOX12C long2 31 10 Analyte 37 022399056 Tox 120 DNO. 115F-G2, 2/22/99 TOX12C long2 32 10 Analyte 38 022399057 Tox 120 DNO. 116 F -G 2 ,2/22/99 TOX12C long2 33 10 Analyte 39 022399058 Tox 120 DNO. 117F -G 2,2/22/99 TOX12C long2 34 10 Analyte 40 022399059 Tox 120, RBL02229-250ppb-CC4, 21 TOX12C long2 35 10 QC 41 022399060 MeOH Blank TOX12C long2 93 10" Analyte 42 022399061 Tox 120 DNO. 118F-G 2,2/22/99 TOX12C long2 36 10 Analyte 43 022399062 Tox 120 DNO. 119F -G 2,2/22/99 TOX12C long2 37 10 Analyte 44 022399063 Tox 120 DNO. 120F-G 2,2/22/99 TOX12C long2 38 10 Analyte 45 022399064 Tox 120 DNO. 121F -G 2,2/22/99 TOX12C long2 39 10 Analyte 46 022399065 Tox 120 DNO. 122F-G 2,2/22/99 TOX12C long2 40 10 Analyte 47 022399066 Tox 120, RBL02229-250ppb-CC5, 21 TOX12C long2 41 10 QC -48 022399067 MeOH Blank TOX12C long2 93 10 Analyte 49 022399068 Tox 120 DNO. 123F-G2, 2122199 TOX12C 1ong2 42 10 Analyte 50 022399069 Tox 120 DNO. 125F-G2, 2/22/99 TOX12C long2 43 10 Analyte 51 022399070 Tox 120 DNO. 126F-G2, 2122199 TOX12C long2 44 10 Analyte 52 022399071 Tox 120 DNO. 127F -G 2,2/22/99 TOX12C long2 45 10 Analyte 53 022399072 TOX 120 DNO. 129F-G3, 2122199 TOX12C long2 46 1 0 Analyte 54 022399073 Tox 120, RBL02229-250ppb-CC6, 21 TOX12C long2 47 10 QC 55 022399074 MeOH Blank TOX12C long2 94 10 Analyte 56 022399075 Tox 120 DNO. 130F-G3, 2122199 TOX12C long2 48 10 Analyte 57 022399076 Tox 120 DNO. 131F-G 3,2/22/99 TOX12C long2 49 10 Analyte 58 022399077 Tox 120 DNO. 132F-G 3,2/22199 TOX12C long2 50 10 Analyte 59 022399078 Tox 120 DNO. 133F-G 3,2/22/99 TOX12C long2 51 10 Analyte .? ConcC C Massiynx - Sample List Sam ple List: C:\M ASSLYNX\FACT-1.PRO \Sam pleDB\022399c.SPL Printed: T ue Feb 2316:25:20 1999 c,, S n ,^ 0 2 D l^ ja a U 6 S/lo/W l . SQf33h<f Page 2 File Name File Text MS File Inlet I Botili oiume Sample Tj Cone A ConcB Conce 60 022399079 Tox 120 DNO. 134F-G 3, 2/22/99 TOX12C long2 52 61 022399080 Tox 120, R B L02229-250ppb-C C 7,2 / TOX12C long2 53 62 022399081 MeOH Blank TOX12C long2 94 63 022399082 Tox 120 DNO. 135F-G 3, 2/22/99 TOX12C long2 54 64 022399083 Tox 120 DNO. 136F-G 3, 2/22/99 TOX12C long2 55 65 022399084 Tox 120 DNO. 137F-G 3, 2/22/99 TOX12C long2 56 66 022399085 Tox 120 DNO. 138F-G 3, 2/22/99 TOX12C long2 57 6 7 022399086 Tox 120 DNO. 139F-G 3, 2/22/99 TOX12C long2 58 68 022399087 Tox 120, RBL02229-250ppb-CC8, 21 TOX12C, long2 59 69 022399088 MeOH Blank TOX12C long2 95 7 0 022399089 Tox 120 DNO. 141F-G 3, 2/22/99 . TOX12C long2 60 71 022399090 Tox 120 DNO. 142F-G 3, 2/22/99 TOX12C long2 61 7 2 022399091 Tox 120 DNO. 143F-G 3, 2/22/99 TOX12C long2 62 7 3 022399092 Tox 120, RBL02229-250ppb-CC9, 21 TOX12C long2 63 7 4 022399093 MeOH Blank TOX12C long2 95 75 022399094 Tox 1 2 0 ,1 06F-G1 -250ppb-M S, 2/22; TOX12C long2 64 76 022399095 Tox 1 2 0 ,1 06F-G1 -250ppb-M SD, 2/2 TOX12C long2 65 7 7 022399096 Tox 120, RBL02229-250ppb-CC10, < TOX12C long2 66 78 022399097 M eO H Blank TOX12C long2 95 79 022399098 Tox 120, RBL02229-H2O B lk -2 ,2/22 TOX12C long2 67 80 022399099 Tox 120, RBL02229-RBUverBlk-1, 2, TOX12C long2 68 81 022399100 Tox 120, R B L02229-5ppb-2,2/22/99 TOX12C long2 69 82 022399101 Tox 120, RBL02229-1 O ppb-2,2/22/9 TOX12C long2 70 83 022399102 Tox 120, R BL02229-25ppb-2,2/22/9 TOX12C long2 71 84 022399103 Tox 120, R BL02229-50ppb-2,2/22/9 TOX12C long2 72 85 022399104 Tox 120, RBL02229-100ppb-2, 21221 TOX12C long2 73 86 022399105 Tox 120, RBL02229-250ppb-2, 2122! TOX12C long2 74 87 022399106 Tox 120, RBL02229-500ppb-2, 2/22/ TOX12C long2 75 88 022399107 Tox 120, RBL02229-750ppb-2, 2 /2 2 / TOX12C long2 76 89 022399108 Tox 120, RBL02229-100Qppb-2, 2122 TOX12C long2 77 10 Analyte 10 Q C 10 Analyte 10 Analyte 10 Analyte 10 Analyte 10 Analyte 10 Analyte 10 QC 10 Analyte 10 Analyte 10 Analyte 10 Analyte 10 QC 10 Analyte 10 Analyte 10 Analyte 10 Analyte 10 Analyte 10 Analyte 10 Analyte 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 000526 Method R eport Method f i l e t L ast M odified! Caopoundi P rin te d ! 0 1\MASSLYNX\FACT-l.FRO\HethDB\022399e.ndb Thu Peb 29 13*25*14 1999 2 t PFHS Wed H er 03 lt* 4 1 i3 9 1999 Compound Monet In te rn a l R of.i Q uantify Tracei Cane* o f S tandardot U s e r RP V a luei UOer Peak F a c to rt I n t e g r a t e Window F a c to r i PFHS (None) TIC Cone. A 1.000000, Disab] 1.000000 2.000 R etention Tine (nine) > R elativ e R etention Tinet T in e Window (w ins)* Peak Selection* 0.513. b a b ie d 0.000, D isabled 1.11? N earest Reopenae Typet Reoponeet Kxtexnal . Areas F o ly n o a ia l Type* P o in t o f Origin* F i t W eighting! A xil Transfoznatieni L in e ar Exclude Mona None U n its* Feak-to-peak asp lltu d es b e e thingi Window s i z e ( s c a n s ! i Muaber o f saooths t b o o t h in g Method* 105 D isabled 1 2 Jo in v alley threshold*. Reduce peak ta ilin g * R aise b a s e lin e naximiwi 30.00 ? o .o o . 4.00 Draw v e r t i c a l th re sh o ld s D etect shoulders* Shoulder threshold* 10.00 D isabled 10.00 R elativ e height* A bsolute height* R elativ e area* A bsolute area* 50.00, b a b ie d 0.00, D isabled 3.00, b a b ie d 0.00, D isabled j 3 j 1 - Soup t a o m i ____ 1AC._ IS3 0 3 m * 3 000527 Method Report Machad f i l a i U a t m odified Ccapeund M afiadt CSu\iKFAa9bSM2W9C\tFfAiC2T9-*11.4TM1)9M9lethOS\022399e.adb It NU Wad Mar 09 2999 Cea^ouad Hanoi QICneucnaaenr,tniafayfi MTStraaaln.daairds User W Valas Usar Feak raeters Integrate Window Faeton JOU IHoo.J TIC Cane. A 1.0000001.000000. Olsablad 2 .0 0 0 Rato&tian Tina (nina) i Relativo Retention Tina Tina Window (aina) Faak Selection* 7.490.b a b la d 0.9020 .0 0 0 , D isa b le d Waaraat i M p c u t Typ B etonai Arana FfoaliynntcaadfaolrTiygpiani* Fit Weighting Axis Tranafonationi Unit a i feak-te>peak a a p litu d e i te s o things Window ais* (aeans)i Wuabar af snoathsi b n n t M n g natheds J a in wallasf th ra sh o ld i Reduce pash ta ilin g A aiao b aaalin a naxinuns Draw vertical thresholds Detect shoulders > Shoulder thrasholdi A elativ a height A baolute height R elative areas A beelute areas 109 1D isa b le d 2 30.00 70.00 0.00 10.00 D isabled 10.00 90.00. b a b ie d 0 .0 0 , D ieabled 3.00. b a b ie d 0.00 D isabled c a o i n _____ l . . - l l c h l 000528 Method Rapare Mathod f i l a i U s e m odified! Co^oundi P riatadi C t\M A IS L Y l \F A C T -l.P R O \IU efaD S \0 2 2 3 9 9 c.n d b Thu Pah 35 132514 1999 4 1 N513 tod Mar 03 K t4 1 i2 9 1999 Coepminrt K o w i In tern al R ef.i Q uantify Traeat Cano, of Standardst U s a r XT V a lu a t Usar Peak F aeto n I n t e g r a t e Window F a e t o n H513 ' (Mona) TXC Cone. A 1.0000001.000000, D isab led 3.000 R eten tio n T ina (mins) i R elativa R etention T insi T in a Window (m ln s )i Peak Selection 0 .(4 0 , Am bled 0.000, D isabled 0.730 W eareat R esponso Type Reapc a s a i A sternal Arana Polynomial ly p ei P aint of O rigini F ie W eighting* Axis T ransform ation* L in e ar A cclude Hone v one U nitsi Feak-to-peak a sp litu d e i IIS A so o th ln g Window s i r e ( s c a n s ) t Humber o f smooths i Smoothing method! D isabled 1 2 Jo in v alley throsboldi Reduce peak ta ilin g ! R a isa b a s e lin e maximns* 30.00 70.00 ' 4.00 Draw v e r t i c a l th re e h e ld t D ataet shouldersi Shoulder th resh o ld ! 10.00 D isabled 10.00 R elative height! A bsolute h eig h t! R e la tiv e street A bsolute a rcai 50.00, Enabled 0 .0 0 , D isabled 3.00, A m bled 0.00, D isabled ( A C O /o i /m Hgt 4 g-fc 0^0529 Method Report Method f i l e t U a t m odified Ccnpoundi P rin te d C\KASSLYMX\FACT-1. PRO\MethDR\033399c.i Thu Feb 35 133314 1999 StM13 Wed H er 03 l i 4 1 3 t 1999 In te rn a l R ef. Q uantify T reeei Cone, e f Standardi U a e r RF V a lu e i Veer Peak F actori I n t e g r a t e Window F a c to r MS13 [Mooe] TIC Cone. A 1.0000003.000000 D leahled 3.000 R etention Tine (aim ) t R e la tiv e R e te n tio n Tine T in e Window ( n in e ) i Peak S e lectio n i P .S fl. tabled 0.000 D leabled 0.730 Reaponae Type Reaponaei e te rn a l Arena F o ly n o n la l Type F e in t e f O rigin F it W eighting i A xle T raaafo n aatio n t Linear cclude Feak-te-peak am plitudei Window a l s e l a c a n e ) t tfiimhsr o f sm ooths! so o th in g atethodi Jo in v a lle y threaholdt Reduce peak ta ilin g R aise b eaelln e m axim al Draw v e r t i c a l th re a h o ld t D etect ahoulderet shoulder threshold R elativ e height A bsolute height R elativ e area A baolute area 1D isa b le d 3 30.00 70.00 4.00 10.00 D isabled 10.00 SO.00, ta b le d 0.00 D isabled 3.00 tab led 0 .0 0 . D isabled p u p . o a o m ___:___ iac m Im / m Page S fJtf . 000530 Method ( l l a i L ast m odified* Ceapeunds P rinted] . Ci\KASILWX\rACT-l.PRO\KethDR\02239Je.mdb Thu Feb 29 13*39sl4 1999 li If Wad Mar 03 14s41s29 1999 Cnagiraind M m i Z ntam al M f.j Q uantify Tracas Cone* o f S ta a d a rd s i U aar RF V alas Uta* Peak Factors I n t e g r a t e Window F a c to r s IS (Mona) TIC Cane. B 1.000000, D isabled 1.000000 3.000 R etention Tina (n in a )s R e la tiv e R atan tio a Tinas T in a Window (m ina) s Peak O alactioos 7.410, taablod 0.000, D isabled 0.90 M earast Rasponee Typos Raaponaos ' In tern al . Areas Polynonial typos P o in t o f O rigins P i t W eightings A xis T ransform ations iln aar S a e lu d e Nans Mans U hitsi -- P sak-to-paak am plitudes IIS ganoth in g s Window a l s o ( s c a n s ) s Msabor o f saoothss so o th in g nothods D isabled 1 3 Jo in v o lle y thrsraholds Raduco peak ta ilin g s R a ia o b a a o li n a maximum 30.00 70.00 . 4.00 Draw v o r t i c a l th re s h o ld s D etect shouldersi Shoulder threshold] 10.00 D isabled 10.00 R elativ e height! A bsoluta h aig h ti R elative areas A bsoluta areas 90.00, Enabled 0.00, O iaablad 3.00, Enabled 0.00, O iaablad Soup. _____ (AC j / j /m -4 000531 FACT: DATA REVIEW SUMMARY FORM De: ' -3 /6 5 / 1 7 , Analyst: / V ) ^ _______ FACT Study Number ~ 7 o k / ? Q Matrix ^A r n Time Points ______________ Dilutions? ________________ Analyte 4: /) S / 3 Acceptable Linear Range: S~D - <7 ^ 0 ^h LOQ for this data set: 6 W C,Q \ ' Re-evaluated for different range? ________ Diiu-li&nc httnA h r c\rp 2 * should d . Analyte 5: /r?6 /3 Acceptable Linear Range: SrO -S U O /y J * LOQ for this data set: ^4 dp'f-i Re-evaluated for different range? Analyte 6: ZZ? jg_________ t>77A- OSSeAV'to*: Acceptable Linear Range: i-A^ LOQ for this data set: Re-evaluated for different range? Analyte 7: _______ Acceptable linear Range:_____ LOQ for this data set: _______ Re-evaluated for different range? Dole.*- (^ftnalgLL -(r fFJiS QrJ. (jilulionj lu Gryj 3 M5/3. 000532 *r- Zi 1 P ve sMsssssslS O HM M nNH h Vi H I II re tnennN tA aeH H HNM AnOIrt SSS99S n^hfii IWI0 9I riri 999999 vi or i nr ivr ii -r o- rniwn rwi nr iwona ririri Mrn twm? imr^ihaAHaonovni rMtHMrOtir.' h4 rinn nI rnini nniornriic*mm ririn9 OnrnNi en<HnONrni0<r4oi 99999 co co h r* si tn rin e nnnn re o ri ro H IS i nrio)ton9 rin n h n ^o n^ nt cr o o nn n i( ^nreitrrti Vr S iili* ri ri 1 n re cv r * ce r 4 ri ri 'f r i r i rihriorriri riri ciroi ti is s ili frii ' n r r ir iN O r ir 1 a r i h w ri M O a n ^ 'w r ir iM M r ir i n S iiiS S ri re i n M *O V H in v i ** r* io a* CO O r i O f# r> n n r ir ir iv SSSSSS 1* ri 1 H r iH H r if i r ih r ir ir ir i m 19 Cri V I *9 f r i 'ri r l r l r i O re ii ii S ii ri0> 19 re i1 O r la lo OOo r if le r ir ir iN H r n r O r i Vi i9 9 o ano re r i re 4 h V r ir i h r i M M J i r> a sa a ss O M C < C r ir ir ir ir ir i w io a M i^ r i r i r i r f ri IV tv v i v i re o v i r ir ir iV r i r i F ^ r i W r i H r i H r i VI v i v i m in a r i t* v i core n r* n n is r ir iH 4 r i H IV re n v i v i nnoe r ir ir ir i ri ri ri ri VI ^ VI vi H e n v i re CO V I 19 99999999 rr iiOoCwO Cr Oi or inO rriiHcViI r i re t i il ii f*i9riivro reri rivto virivivireri ^ t s rriem^r inoc on^cvcoonvr ii ovcoi ar i ^a on irnriirrarliirWvri-rai^Or aer Oirneri r i re ri b se eo a R1I e v e o o c o m v io v tv iin e o o o e o r io o e nnnnnnnnnn aaaaaaaaaa 00 00 00 00 00 90 00 09 00 m om oooooo r i r e m ro mre ion mr - oo 9v i e o in re r9 vi ri vi n re re r i r i o o . 999999 ri ri re e re r9i ri o r9i o VI 9r i VI ri o aaaaaa r i r i o io e u vi ia r n r* n *s v9 r r- r r oo 99 * e o o m Oo in m re re r i fV t r i CDIV r i rrei n9 O* nO On iVni aaaaah r in r iv n r1e-1^9 n0 0"V 9r i 9n aaaaaa re r i re r** re rrei roi r9i rOi iVnI o** n o o ro in Hr i ritn Ar i Or i OrcioO9o in qr i anaaa Vr iI V9 r10i 9r i 9r i rei 9 VI O O 9 VI 9 f 9 9 9 r r9i 99 9 ri tn r i O VI VI VI 9 r* r* F"* Vi Vi Vi r9i VreI VreI 9 r* f* 9e o o oo o o o o oo o e ri rio in re 9e re o re o ri re o 9. o n tn re re re e r i'V f'ririre rirc ri re riririririririv i e e e io c t o c ic ie c i 9 9 h n F > F 'a r 000000900 o o o eeo o o o r i roi nr i roi oo no oo i on oo r i re in r* o n_ CO IO o o o mm_ .%%%% Jj X i V Al sssss ssssss ssssss ssssss s a s s i slisss IllIlllllIliIllIlSalialalllllalIllsIIflIlB lIlIilsIIIlslIIslillslllsl 9 a ftei Ih I ri re vi v i re vi vi vi vi w s s rimririririris n n vriririssssn res ns snsnsnnnnnnnnnns n rin n n n ssssn in sssn n n n M snnn n hn * *n i ri n n n n i M te n n n ; V tii 3SSS o o o o o H Kn Mr iDHrrai rOi rr iinOr ri hi rOi nVI InV InCI InVI lnVI lnVIlVnIlOnIlOnIIVnIIOn II nnnnnnnnnnn 3n nO nQ nO nO nO nO nQ nO nO nO J JJ J J JJ SSSSSSSSSSS HOOOOOOOQOOO R nr i nr i nr i nr inr inr irr ii irii rr ii rni rni mmnm 1 i 9. a i evni 0 1 * 1 P > W ! p o p n * 3 T 4 < TM nfc ' T O Z O n o ssassassssssssssasssssaaaaasssassxassaasasasaassssayaKasassssssKassKssssKKaaaas..| C/SE/Z ltd Coaa lasaiass sssssssss iiiiiiiii a a ss a s 9tAt A 4*1 ssi i ii i a s o i sil o o lIlsS a s o en 5ssSssco CO US5SS2SS > MUwm M<40 iiiiiiiii Mw i s as IS s. h t asa 5 oo So sbs a ss ss oi A Ul A i * M ggg g gg SS o So i asa i w w g . ggg a s * a 1 s a i, Kl g aa 5s A * *1A A i a ii i a 3 <4 A si I a as i 5M o oo s SS a 1i W a H -* g g gg g s S o" sa t * - gg a s A A*4 i ii 3 ; ' ISsaSsKs s sssssssss rra r r r r r r r r r r r ats s ssSassScsS 3 i as S So S SS 1 u A g gg l is a Il3ll=HS sao ass 1 HA ggg A asassaaoa u asaassssas i i iw III 1 MMW ^wHfcotoau u g gggggggggg * s i ss L s53s:;2ss?ssss:a2s^s23a522E?ssa3SS2i5Bsss:5:s;r;sssts;si:sKt:sss3SSiiSK;t:s;s5:sKts---i.u.^l.k.>.. iSSiieBilBfiBBeBBBeEggSBBeESBBSeSBeSISISBBiSSSBIBBBSiSiBSISSBSBBBSSBSiillil 1 sssssssasssssasssss S3SS2SSS1SISSSS2|S iilliiiiiiilllifiiiliiiiliiiiiiiiliiiiiiiiiiiii V 1 !p !1 fofff Si mmmmmimnmmimmimmimmimmmmmmnmmmmmmiii g s S s S S S S s S e S S S s s S s S S s S S i ^ S s s S s S e S s SPSSSSsSfSJSS5SSSsSsssSgSSSSsSSSsS^Sg^SSSsSSSgS8^g3SiSS! [{ If k ks S S S i;lSlSiSisi-lilTSs5 l'*nn\nn'*ni'znn'*nw 5|gS p p g p s p p i s m }352 f sss sssss sbbhb ssf i s if# I#i sssssSiih; , ssSs SSSS"S ms 2r3! i ili! l,,... acLa^a^P-P. issalsasu. sskissssi B ss ss *4 S Sg Ss sgg sss 4ggi4<) *4g i g g g g a S S2 SSHS S W' 5 O O O SSsSSa i=l i C/T CO S2K5S3S C/ sbbssisb * ***i* gglIVIII. i HB s a a s s s 3s S SS SsSsSS 53 g 36 833358 S3 s sSSs ssSSsS S 3 .2652 SSS325 5 855522 256258 6 g igsgiggg s 2SSSSS8SS IgiSasgs P SsssSts. S 8355SS83 ggssssss s? swm Soup 02019911 qunatltntod and printed fay m 3/25/99 saasasasssssssssasssaaassaapsssaxssaBBgsasaaissasssygKiiaKSgsssKKSSKSEiitJi:!: rasas., ss :sssi:lli| | | ll ll! il l ! | ! ! i| ! i ! { ssils 1 i S 3 Isss i mmmmnmmmmnmmmnmmmmmnmtinmimminmmmii ESSSSESSSSESSSBSSSSiSSSSSSSSSSSSBSSSSSSBSSSSBiSSSSSBSIiSSSsSSSSSSsSSSSSSsSSSSSSSSSSSsg ;'B;v3'I;':',;'B(',;;i;!(ii;!)ii!i;iiiiii'eiS88!E'c|j|ggrl!gi|{mipgi:igsiiiegg|g|iS8 g s g g h e.B.SSEi:iS(i miiiii i l l l l l lilis lili! il I .U :hikh l ili p i l l i [ H i l l SS PsSSSS "sssss Usi m i? m iiiiiffii SSSS Is ls s s s s . S .g g g g s s g ss'sssssss s s s s s s s s iiiiii SS i i i i i i iiiiSS SSS3 i i gsisss asaSs kvs sksbss SiidiK gXXXXX tU BaseSssssE SSSssii ssbI ss slssSa s l l s S SES ssSs s iiS 55sls s s l l l l S lls s s c l l S I l S S 3 3 SSSS S S S S S S SBSSBK S3XSSB gCSSKK S B S S S S a LL C 3 s SX? XSXS XEKXXX H f f B W ififSSSS ISSSXS XSXSSS uI> S 3r3vc stsSssssssssssss lililili jj ! s SSSHssas sasssago sssasass .. a H I M h* U O OMMMOHHO gBSSSESS S e ? f < I s s I H* *I* t R& ? I oooooooooooooooooo >000000000000000 oooopopopppopppppooopoooppooooooooo* tMOl OI-OOlMVOIHO OH> WOMOWMiHOHOt f0Vla-W<lMOAO)I0IOIV^Ol(iOei MWO OHi OeO(Ol(tllO*( l>OgaO>nUOMIOM OUa iMOl COHlOO^ >IOOJO>OJOI>OjlOAi 'UO>IOl ^>JOWs lO*MJOH<O4OOO)(OOt >tOJAOOAi UOOIO(#AlOUAOMAOAHAOOUO* IOOUIp,>UO*(JOMOpIlIVU^IWU lMi fHl U^OUI(l *^ J O t Of kOl t Ol kO^ fOk ^OWOWOKOWOWOWOWOWOWOWOlOi l OWOMOMOMOWOMOMOMM i m t2S33g3g?38 XXXXXXXXXXX Sx ix?!i Itm aa P H H H H H M H H H r - H -** M N N IMIMN N IWmV MN MN N Vp V4HMMH OOOOOOOOOOOMOOOHOOO * >> HX0* HH O 0O* HHHH WMMM OOOO 0 MUMHWM HOOO HN MH OO HM O 0 MhWw HOO Mm O mU O i m m i t m m m m m m i m m i m m m t t ia as HPHHHH. ** "* *m 0 K1N MMMW0 HM Hb MHWHHU HMHMMWHWMW X X mf HOOOOOOH O H O O O O O M O O O O O O H O O O O O O H OOOOOOOOOOHMH ssesssesse* PSIM0 r 'Oh Oh MOOOf t0Op0Op 0Op 0Op OtO' o $ Q ! l l ! l I? l i l i ^ i i n i t ' i IsS iiS il MU MMMMMMMN1.N....N....M.....M.....M......M............M.....O.....A. UMMMMNMMMMM MHH t0 IOWA O I I I III Ililil I MM s s s ls S S0 8SH4MM ow ovo K S t f g i S MUM MO O O OOOP IW Wvr7?-*s& I r r1 MNN* HK EssMIM W N* W* M H, .M n o * NKHKHH MWUWUU MWU U U U bu ao ub WHU SMSM*Uv MMW Ws iUt Ua ka l Up Uh h l . 01 f o uowwww o* * * MNMMM &SSSSH T mummw nWMMMN fJSNSSS 3 MNWUM fi' N S N S V i mmmmm nQMNMsMs Ms Ws mhhm MMMM ----W-- sl*O- tWU ssss 0* * * S UN W D, ' * ' * S ( UUM OMUM O *s. *>s*s MMNMHH KI MHOt t M a *8* *8*8*8 lilil MflOQA Uoi*UMM*N*n fWMMNM SSVSV NMMMM qmwijmw m ili iiiiii 8k .s..s..s..s..s vMWMMM 0` s . S V S S 1 MMMNM nUMMHM UMM-S Jf* MMMM N N S M I H* O 01 aaa aaa aaaaaa a a aa a 3a a a a a * aaaaa a a a a 100 WV aaa W ' ^ ' . S S WWNMHW MS SMWMM MMMS< N SN MMMMM s s n m m MMW NSNSV. U V t f 4 NM s . UWt A<0 S N (Al AtttfV Mtt Wt f t t N Mi VIA 10 S- Ui HfHf )HH> MMMW . 's s s s I MWWM UWIAI d l lfp ig l g* - ` W>0MHoHaHH s MM OHOHWM *tlt 1 Ii ooo MOflHHH WH H* * OWOMOMOWOHONMOMO WD OWOU MMMMMMNMMMM tMIS tNIf tMI0 tMId lMI NI0HWI MUIM>IVM0I MWI oH *u JiUoMu HoUoI uWpHiU U) 8D 0 0 Ooes S S Ur 0 fMMMMM SSSXS MMMMM " " MMW MUM WMsvs NNMMM Tf HHH HB W0WI0WOWV0W iMMMUU i htWi MS N ' f c WWm * WMMUNVSMI r t N \ MSSSSMMMNHH i SHMMNMMNS*s MHWMWSNN H M S S ^ N VIOWIAMM Su)0I' O100tyfWWtf S\ MIA 10 k) 0 IS ff l B55 *1 I i fl O o o C/l co OMUl WM OUI OUOI MI H OOOOOOMOI l I 0 ^ IX* XV XV Hf V* XX* W+ , H*J ^ )*jnui 0M ew ve m #10 tAWt0 UWW0 a a 1 01 M0 0 l 0 10 10 10 10 10 *U 0> 1 -j 0 j (0 10 10 O(0 VA 01 aae nafa 10 10 1A10 <0 10 10 10 10 10 10 10 K>H H Of JHWMH I OM0 0 A 0 W0 0000000110 y a tauiu a m h u m m u u j SSn 0 aa amow u0 00 wwUaSSS u h 0 h a v m m m u m n w m m w w m u w u 0 0ij0o0O ow hohm 0 h 0 h u 0 oi u > m a a 0 w i 0 h ma a mm 0 00 0 h 0 mhwmou ** <4 HA w- Ig0AMHHU N UttHURMHa BI WB^WWWWI - MWU HHU WW*J si | nI 0^0 11 y y B 355 0*100 5m *h |J *4 - 533B HUUJJ o SSShm | 5&5&&B sj*i0B o w tta w u w u S a o CawS*-* 1 "'`' W H SI . 5 & m & B3B5B5 0 H HM aaoaoo H0MWW0 0 0 0 UWU aoaaaa UHHHHM MHH0MO1 a a w 01 0* si 0*1000 mooumou M m KI m 1 I M Ix a M 5 & m B BB&B&B & I a ? Ooo iuol Uoo aNo oHoaoMa Ho t aaaaaaa I000HMOAW0 WHI oaaa aa c 0a iHal UHa MuUHw0 0s i 53 g g m iv 3 s Is f m f H H E H H H H I H I H Z E H H H IOUHIUIMHMMIUBfI m m n m \Mff 0 WH MH MP MH MK HM t HOOOOOOi MM MH UM D-MM MM 90 0 0 0 HhHHHM HOOOOOOH UMMMVMMMMM OOOOMOOOOO. immi nMuOtjOMOMtOjOtOlMlMe oWoMoMeMoMeWeMoMoWoMHtIHVH* & I 538883'oMp Mop Mro MPo fWo rMo 1& MKl(IMiMlNWHtiMUHt-lMWWgtMMgt g PO ? ! JsJMnMUNMMvMSMMMnlSWJMMNI's4 4 4 4 M MM MNN IJPPMHH h ro*m \ UN UoWl QWU4HiAWUOl1)WUi*^O0lUU*mf Uw Wl*4 <mMM0Uk*MUhjIWhM*bhH*l*hOU* m w Sww IMMWMM I MMMMM 8; f'llSII1 m H m h i i ligliUli .................... & S ............ M M H O 4 (B .UJfnIIfMMNS 4SMM4MNS4IM4MNS4IM4MSV4M M4USN4M ioMiHuiHmIi I " * " I0uJdi")m"mi"lm "Cm1 S 1 MUMM kM MMM O HHp H HPO i HO4 n HO4 * Wf)f> MHH 441IMMM<4AOO41U1AO*I*1 *> MOMOHOH4444-J *I MVD*H4 *044i4 < 4I i M2n M *JUl |J H W 0 m o ut o o m < 65I`SMN.MMS.MMX'MMs 8MWNM W 4 4 4 4 I MMMNN Qtro'crtri iY--* MN*SI M M I N4 Nir' aT * M M4UNH 4MMS4 MS44 WSW4 WS44 4 o* Y Y Y Y * * * * * * * pe A1n*M* -* M * * M ** H *** NM NM * SM MsMKIHH*HI SmMMS4 MN4M4nM4V4WxHK4Ms4MsV44MMm44NMm44VM ms44> .n44 *h MSM MmMSVMI ta uui tii n * !i3S?3li~R *Ss1g* t n n si H 4 M ? *?fi &W IwJjKMjH *mBKH f ?3i3 SI ? S??88 3 A HHMH :44- m4:"^ggio4:m"g?o1^sr 8 gigggigggSi?si!i8E B E si n n B.&Z UuO MOm MO4 WO4 WO4 MOU MO4 MO4 MO4 oo oo oo oo oo oo oo oo oo Mme Moo oo- `oo MUOl oo Mmo oo MUOl Muo oo oo 4 -Jsi>1 >41-1 4 >J1 4 4 0 M4A WMWUMUl tMWtM4A *MWlMUU IW4WHI AW0 MUOA E4 4S 4K 4 4 4 4 <4 <4 <4 J <4 *4 1 4 <4 *i4 Ni 4 *4 Ni <4 nJ <4 4 4 4 4 4 4 MU4 NWIN44 W4K) WmVSWmlW4m MOu W4u H4 U0i1,tU0JUMUWUMUWMB HUU UMm Mw a WuWH4Wwa* e> MHU SMU UUMMWMIUMi UMM 4iOd OO 444444 MUW MU4 WMU MU4 UMH AHO MMO UMOl' Oo oa 44444 uIA I^wU4uUUKwIImWU 444444 MW4 UWM M4WUWMUMMf 4Ut WMO oo . 444444 U4A WHA lMUiMPW4NA 44U MIodUMol MoU MoW MoU MoW MoUlMolMou oo oo oo oo oo oo oo oo oo 44444444444 M4 oMmWmUm mW mOw WvUoIiUoMw*> o o o CO 00 44A44R404UW 4 AA4UIHI0H AW4 OURHORU4IIIHM 4ldU 4 AO OI Ni O 44 AW 4AU04U OO140* 4 N 4 U U U H 4 Ow A A A l i AW a m o m a U 44ROAU MUt O011410 WAUUO OUl HO WU OOOAAO A A4A4W WOA A A AOOB4 400400 UMU0UO O4H004 O O<4O14 AOUH0 OWO 140i 4 0 O0 0 W W4 W4 IdA HOWOWA M 10O1010t001 OH M0 4 O 001410 i ill 4 4 4 4 4 0 4 4 AMM OA 4 AOUIOA0ON A MOOAWA A 0 0 A NMMMMMMMIJ M mmoummui*W I44AWW4UI0 aMOUl>M0W>JOUA W04H04RmAAH MH 4MOO H 1410 0400 HAU MMMH MNOH 4 0 AH 00 WOUO NMHHH UOM0UH HO4AO0 '4 ' 4 n ( ll W0 I H4 UA 1 1h i 11 1 OIR ohoiuw aw rhw m 11 MO HAO 55555555555 555 f1 1 1 HU N U 5555 III 1 HMN 1U HNUHU0 555155 MWMUHH 04UB0M H40U0A HWNO0N WAOUWA 1 II MH H H OHAuao 515558 HWMUMH U04HAN O H W HMUHWH HAUHU i O H 0 U H 555555 4MHMMH 4H0H0M 0UOOUA U4004M WH 4 A O4 0J01010) 0i M A A4A4W W0040O 00OOH WH4U00 MWMWH *4Ul A 01M 0 1A011414 0 OU A 4 0 4 OOA MM14M01M W0O04H 4 WK) WA 0 o o Ino *i o OWOiNOH 141401WW01 MMOMHM H 4 O0 A W O010101014 0 4 0 AA NMMMMMMMM W0W0W4WAMO4 4 M A4A0HOAM MHbwAAW0A4A AHW0WWMA4AA 111 H 1H 1A B H A A MO 555555 1 H l H W40HH 555555 1 MOI Ut 1 HWHHU MMMUt O u A H A H 4 55555 555555 1 0>140*0H CB* * o ON| o 555555 111 1 1 M 1H A4 uhhhuhw w m hh 55555555555 3 g Q u a n tity C a lib ra tio n h a p o rt T e n 1 3 0 EN0> S a t L i v e r B c t r a e t a C a lib r a t io n : C: \KUat.not\rACT-l.T*O\CurvaI\022391a Lent nodlfiad: Thu yak 23 13:43:3* lift t r in t a d i Thu Tab as 13:13:33 139* lag s 1 Q u an tify C a lib ra tio n la p o x t T o x 13 SNO, K a t U m e x t r a c t a calibration! C:\MuMMllX\ncs-l.mo\CurvaPa\033399a tant aKxlliadi O rob 35 13:43t3l 1 rrintad! tbu Tab 35 I S iMtSS 1555 ay a g a Soup 0301951 > q u a a tlta ta d an d p r in ta d b y a a a 3 /3 5 /9 9 000540 Q u a n tify C a lib ra tio n JU port S e x 1 2 0 ZWO, b a t t i r e r d e t r a c t a Calibrations Cs \MLBSLYHX\raCT-l .n o \ C u r r e C B \ 022399e Last nodifled: Thu Feb OS lOtiOsOS 1999 Tinted! Thu rab 25 13t43tS5 1999 Soup 020199t! q u a n tita te d an d p r in te d b y n e e 2 /2 S /9 9 000541 Q u an tify C a lib ra tio n lo p o rt T e n 1 2 0 OHO, R a t L i v o r e x t r a c t s Calibration: C: \IOJiLa\FlCT-l .FR0\C u m B \ O 2 2 3 9 9 o Last aodiiiod: bn Fob 2S 13:43:3 1999 Friatsdt fbu Fob 25 13:43:55 1559 Soup 020199:: q u o n tita to d an d p r ia to d b y ano 2 /2 5 /9 9 000542 Q u a n tify C a lib ra tio n lU p o rt T o n 120 SNO, B a t t i r a r B n tr a e ta Calibrations C: \XxaSLYt0C\riCT-l VftO\CorYal\02239o tarnt aodifiads T bu fab 2$ 13:43i20 1999 Trintodt Tbu Fab 2$ 13i43sSS 199 p as% 5 Soup 020199s * q u a n tita ta d and p r ia t a d b y n aa 2 /2 S /9 9 000543 Q u a n tify C a lib ra tio n X aport o n 1 3 0 SUO, H a t U w a t t r a c t s callbrat Ioni Ci M o a s u n a i r a c z - l . m o \ c u m \ 0 3 3 3 33e Last sndlfladi Thu Tab 35 U i U i S l 1*5* Prints*: Thu rsh 35 I3i43i55 15 paaa f Soup 0 3 01$S :i q p ia n tlta ta d an d p r in te d by 3 /3 3 /3 3 000S44 Draw v t f t i e a l e lu ru h o ld t Daeaet ahouldara i flfcouldar th resh o ld 10.00 D isabled 10.00 0eI.eS0eSSc S iS i m IT IT *e o o* oo / 00054S M i t t'St'tt St K U nwBtccttoNKnnHvmi'i-xsviMnoivniiX'a l*TJTP" I t u p r * od.* poinw SO U P 020199: F A C T E q u ip m en t L o g 99014 Q uattro II, #6414E P A G E _______ DATE: 2/24/99 ANALYST: drb STUDY NUMBER:Tox-120 MATRIX: R at L iver___DESCRIPTION: Liver Samples . FACTM ethod: FACT-M-4.0 , Injection volume: 10 uL Cycle time: 13.5 rflin. Electrode: Z-Sprav______ M obile P hase: (A)2.0 mM NH4CH3CQ2 (B).M s.QH _____________ TN-A- or stndrd number (A) 98012-1-4 ___ (B).XN-A-22$Q_____ ____ Prepared (date/by): (A) 2/11/99 hoi________ (B).2/29, h o j ______:____ Expires: (A) 8/99______ . (B)_3/22_______________ Storp at room temp? or N Other:---------------------- -------- :-------- G uard colum n: None________________ i_ P art number: na______ __ L ot number: na ________ ;____________ A nalytical colum n: Keystone B etasil ______________________ Size: 2 x 100 mm_______________ Type:_lS____________ Sphere size: 5 um_________ P art number: 105-701-2__________ Lot number: P8C09 Serial numbcr:lQ8811Q6D A nalytical param eters: Drying gas (L/hr): 300 ESI nebulizing gas (L/hr) 15 LC Flow rate; 300 ut/m in . B ackpressure: 120 bar Sheath gas (Uhr)_Q_----- H PLC solvent gradient: Long 2 Tim e fm in.) D000 2) 8.50 3) 11.0 4) 12.0 5 L 1 3 J______ J& 2-----------------M Q ___________ JLQ______ :____ 90.0___________ J fl.iL -_________ Mm_______ 000546 Tuning Method Report Method: C :\MASSLYNX\FACT-1.PRO\ACQUDB\PFOS Printed: Wed Feb 24 15:22:59 1999 ' r .. ____________ _________ Spuj._&a.0M__ lA<L QS/fofo Page 1 ;,w r m w u SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. Set Rdbk 3.00 60 5 0.2 150 250 2.99 -60 -7 .150 250 Pressures An*alyser Vacuum Gas Cell . Rdbk 1.2e-4 5.2e-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^ 2.0 " . 0.0 53 650 Set Rdbk 15.0 15.0 45 2.0 0.0 40 0 650 42 38 42 000547 g c u n i n g Machad lupore Maehodi C t \ M M * u a c c \ n c T - l . m o u c a o s a \ T a x l 20A L u e Modifldt Sua rab 33 10:01:03 13*9 P r i n t ad: Wad F*b 2 15i23:l( 1399 elvant Balay ( ala ) i 0.00 Function t 1 MRM et 3 M a u Pair. ( Xlf- } Inter Channel Delay ( Sees ) x Spaa ( Daltons ) t Start Tine ( Mias ) s Sad Tiae ( Mins ) i Repeat* * Channel Parent Daughter 9.03 0.00 0.00 13.50 1 M l (Se.) Coll i n r g y (.V) 1 399.00 30.00 0.25 2 399.00 99.00 0.25 3 399.00 130.00 0.25 43 45 43 60 60 60 <V.) Function i 2 M UM of 3 M u a Fair. (. ZSP- ) Inter Channel Delay ( Sees ) i Spaa { Daltons ) t Start Tine ( Mias ) i Snd Tiae ( Mins ) x Repeats Channel Parent Daughter 0.03 0.00 0.00 13.50 1 Bull (Sees) Coll Bnergy * (.V) Cone ( V J 1 499.00 30.00 0.25 2 499.00 99.00 0.25 3 499.00 130.00 0.25 43 45 45 60 60 60 Function i 3 MUM of 2 M u a Paira { SSF- ) Inter Channel Delay ( Secs ) t Span ( Daltons ) s Start Tine ( Kins ) i En d Tiae ( Mins ) * Repeats i Channel Parent Daughter 0.03 0.00 0.00 13.30 1 Dwell (Secs) Cell Energy (VJ Cone { v 1 1 299.00 30.00 0 .2 1 2 299.00 99.00 0.25 43 45 33 35 Function s 4 M XK of 3 1toss Fairs *{ ESP- ) . Inter Channel Delay ( Sees ) i Span ( Daltons ) Start Tiae ( Kina ) x Knd Tiae ( Mins ) i Repeats Channel Parent Daughter 0.03 0.00 0.00 13.50 1 Dwell (Sees) Coll Energy (.V) Cone ( V ) 1 413.00 119.00 0.23 2 413.00 169.0 0.23 3 413.00 213.00 0.23 30 20 30 15 IS IS Function x S HIM of 3 Mess Fair* ( M l - ) Inter Channel Delay ( Sees ) i 0.03 Span ( Dalton* ) * 0.00 Start Tiae ( Mins ) t 0.00 Snd Tine ( Mina ) 13.50 Repeats t 1 Channel Parent Daughter Dwell (Sees) Coll Energy (.V) Cone < V ) 1 > 469.00 169.00 0.25 2 469.00 219.00 0.23 3 469.00 119.00 0.23 ' 45 45 45 30 30 30 Faction i 6 MRM of 3 Mass Fairs ( ESF- 1 Inter Channel Delay ( Secs ) x Span ( Daltons ) t Start Tiae ( Mins ) i Snd Tiae ( Mins ) Repeats i Channel Parent Daughter 0.03 o.ao 0.00 13.50 1 Dwell (Secs) Coll Energy t.V) 1 369.00 169.00 0.23 2 569.00 219.00 0.23 3 369.00 119.00 0.23 43 43 43 Cone C V ) 33 33 35 Faction i 7 M R M of 1 Xkta Fair ( tflf- ) Inter Channel Delay ( Seca ) i Span < Dalton* ) ,t Start Tiae ( Mina ) t End Tiae ( K in s ) $ Repeete < Channel Parent Daughter 1 427.00 10.00 0.03 0.00 0.00 13. SO 1 Dwell (Sac*) Coll energy (eV) 0.23 40 Cone ( V ) (0 lAL or/hli 000548 '*kr: >>n 1 M asslynx - Sam ple List Sample Ust: C:\MASSLYNX\FACT-1 PR O \Sam pleD B \022499a.SPL Printed: W ed Feb 2 4 1 5 :2 5 :3 9 1 9 9 9 _ ,,, / Soup P1QJ31. JAC Ql/Io Page 1 F ile Nam e File Text M S R ie In let 1 B ottk olum e Sam ple T j C one A C o n c B 1 022499001 MeOH Blank TOX12C long2 91 10 Analyte 2 022499002 MeOH Blank TOX12C long2 91 10 Analyte 3 022499003 Tox 120, RBL02229-H2O B lk -1 ,2/22 TOX12C long2 1 10 Analyte 4 022499004 Tox 120, FtBL02229-RBUverBlk-1, 2, TOX12C long2 2 10 Analyte 5 022499005 Tox 120, R B L02229-5ppb-1,2/22/99 TOX12C long2 3 10 Standard 6 022499006 Tox 120, RBL02229-10ppb>1,2 /2 2 /9 TOX12C Icng2 4 10 Standard 7 022499007 Tox 120, R B L02229-25ppb-1,2/22/9 TOX12C long2 5 10 Standard 8 022499008 Tox 120, R B L02229-50ppb-1,2/22/9 TOX12C long2 6 10 Standard 9 022499009 Tox 120, RBL02229-100ppb-1,2 /2 2 / TOX12C long2 7 10 Standard 10 022499010 Tox 120, R B L02229-250ppb-1,2 /2 2 / TOX12C long2 8 ' 10 Standard 11 022499011 Tox 120, RBL02229-500ppb-1,2 /2 2 / TOX12C long2 9 10 Standard 12 022499012 Tox 120, RBL02229-750ppb-1,2 /2 2 / TOX12C long2 10 10 Standard 13 022499013 Tox 120, RBL02229-1 OOOppb-1,2 /2 2 TOX12C long2 11 10 Standard 14 022499014 MeOH Blank TOX12C long2 92 10 Analyte 15 022499015 Tox 120 DNO . 145 F -G 4 ,2/22/99 ' TOX12C long2 12 10 Analyte . 16 022499016 Tox 120 DNO. 146 F -G 4 ,2/22/99 TOX12C long2 13 10 Analyte 17 022499017 Tox 120 DNO. 147 F -G 4 ,2/22/99 TOX12C long2 14 10 Analyte 18 022499018 Tox 120 DNO. 148 F -G 4 ,2/22/99 TOX12C long2 15 10 Analyte 19 022499019 Tox 120 DNO . 4 9 F -G 4 ,2/22/99 TOX12C long2 16 10 Analyte 20 022499020 Tox 120, RBL02229-250ppb-CC11, i TOX12C long2 17 10 QC 21 022499021 MeOH Blank TOX12C long2 92 10 Analyte 22 022499022 Tox 120 DNO. 1 5 0 F -G 4 ,2/22/99 TOX12C long2 18 10 Analyte 23 022499023 Tox 120 DNO. 151F -G 4 ,2/22/99 TOX12C long2 19 10 Analyte 24 022499024 Tox 120 DNO. 152 F -G 4 ,2/22/99 TOX12C long2 20 10 Analyte 25 022499025 Tox 120 DNO. 153F -G 4,2/22/99 TOX12C long2 21 10 Analyte 26 022499026 Tox 120 DNO. 154 F -G 4 ,2/22/99 TOX12C long2 22 10 Analyte 27 022499027 Tox 120, RBL02229-250ppb-CC12, TOX.12C long2 23 10 QC 28 02249928 MeOH Blank TOX12C long2 92 10 Analyte 29 022499029 Tox 120 DNO . 1 5 5 F -G 4 ,2/22/99 TOX12C long2 24 10 Analyte 30 022499030 Tox 120 DNO. 157 F -G 4 ,2/22/99 TOX12C long2 25 10 Analyte 31 022499031 Tox 120 DNO. 158F -G 4,2/22/99 TOX12C long2 27 10 Analyte 32 022499032 Tox 120 DNO. 159F-G 4,-2/22/99 TOX12C long2 28 10 Analyte 33 022499033 Tox 120, RBL02229-250ppb-CC13, TOX12C long2 29 10 QC ' 3 4 022499034 M eO H Blank TOX12C long2 93 10 Analyte 35 022499035 Tox 120 DNO. 1 6 1F -G 5,2/22/99 TOX12C long2 30 10 Analyte 36 022499036 Tox 120 DNO . 1 6 2F -G 5,2/22/99 TOX12C long2 31 10 Analyte 37 022499037 TOX 120 DNO. 163F-G5, 2/22/99 TOX12C long2 32 10 Analyte 38 022499038 Tox 120 DNO . 164F-G 5, 2/22/99 TOX12C long2 33 10 Analyte 39 022499039 Tox 120 DNO . 1 6 5 F -G 5 ,2/22/99 TOX12C long2 34 10 Analyte 40 022499040 Tox 120, RBL02229-250ppb-CC14, TOX12C long2 35 QC 41 022499041 M eO H Blank TOX12C long2 93 10 Analyte 42 022499042 Tox 120 DN . 166F -G 5,2/22/99 TOX12C long2 36 10 Analyte 43 022499043 T o x `120 DNO . 167F-G5, 2/22/99 TOX12C long2 37 10 Analyte 44 022499044 Tox 120 DNO . 168F-G5, 2/22/99 TOX12C long2 38 10 Analyte 45 022499045 Tox 120 DNO . 169F-G 5, 2/22/99 TOX12C long2 39 10 Analyte 46 022499046 Tox 120 DNO . 170F-G5 2/22/99 TOX12C long2 40 10 Analyte 47 022499047 Tox 120, RBL02229-250ppb-CC15, TOX12C long2 41 10 QC 48 022499048 MeOH Blank TOX12C long2 93 10 Analyte 49 022499049 Tox 120 D NO . 171F-G5 2/22/99 TOX12C long2 42 10 Analyte 50 022499050 Tox 120 D NO . 173F-G 5 2/22/99 TOX12C long2 43 10 Analyte 51 022499051 Tox 120 D NO , 174F-G 5 2/22/99 TOX12C long2 44 10 Analyte 52 022499052 Tox 120 DNO . 175F-G 5 2/22/99 TOX12C long2 45 10 Analyte 53 022499053 Tox 120 DNO. 177F-G 6 2/22/99 TOX12C long2 46 10 Analyte 54 022499054 TOX 120, RBL02229-250ppb-CC16, TOX12C long2 47 10 QC 55 022499055 MeOH Blank TOX12C long2 94 10 Analyte 56 022499056 Tox 120 DNO . 178F-G 6 2/22/99 TOX12C long2 48 10 Analyte 57 022499057 Tox 120 D NO . 179F-G 6 2/22/99 TOX12C long2 49 10 Analyte 58 022499058 Tox 120 DNO . 180F-G6 2/22/99 TOX12C long2 50 10 Analyte 59 022499059 Tox 120 DNO. 181F-G6 2/22/99 TOX12C long2 51 10 Analyte \. 000549 Masslynx - Sample List Sample Ust: C:\MASSLYNX\FACT-1.PRO\SampleDB\Q22499a.SPL Printed: W ed F eb 2415:25 :3 9 1 9 9 9 ,, ni..e...l..l...i. lA c.nsll.lv Page 2 File Name File Text MS File Inlet I Botth olume Sample Tj Cone A ConcB ConcC 60 022499060 Tox 120 DNO. 182F-G6 2/22/99 TOX12C Iong2 52 61 022499061 Tox 120, RBL02229-250ppb-CC17, TOX12C long2 53 62 022499062 MeOH Blank TOX12C long2 94 63 022499063 Tox 120 DNO. 183F-G6 2/22/99 TOX12C long2 54 64 022499064 Tox 120 DNO. 8 4 F -G 6 2/22/99 TOX12C long2 55 65 022499065 Tox 120 DNO. 185F-G6 2/22/99 TOX12C long2 56 66 022499066 Tox 120 DNO. 186F-G6 2/22/99 TOX12C long2 57 67 022499067 Tox 120 DNO. 187F-G6 2/22/99 TOX12C long2 58 68 022499068 Tox 120, RBL02229-250ppb-CC18, TOX12C long2 59 69 022499069 MeOH Blank TOX12C long2 95 7 0 022499070 Tox 120 DNO. 189F-G6 2/22/99 TOX12C long2 '60 71 022499071 Tox 120 DNO. 190F-G 6 2/22/99 TOX12C long2 61 72 022499072 Tox 120 DNO. 191F-G6 2/22/99 TOX12C long2 62 73 022499073 Tox 120, RBL02229-250ppb-CC1, 2/ TOX12C long2 63 74 022499074 MeOH Blank TOX12C long2 95 75 022499075 Tox 1 2 0 ,1 10F-G1-250ppb-MS, 2/22/ TOX12C long2 64 76 022499076 Tox 1 2 0 ,1 10F-G1-250ppb-MSD, 2/2 TOX12C long2 65 77 022499077 Tox 120, RBLQ2229-250ppb-CC2, 2/ TOX12C long2 e 78 022499078 MeOH Blank TOX12C long2 95 79 022499079 Tox 120, RBL02229-H2O B lk-2,2/22 TOX12C long2 67 80 022499080 Tox 120, RBL02229-RBLiverB!k-1, 2 TOX12C long2 68 81 022499081 Tox 120, RBL02229-5ppb-2,2/22199 TOX12C long2 69 82 022499082 Tox 120, RBL02229-10ppb-2,2/22/9 TOX12C long2. 70 83 022499083 Tox 120, RBL02229-25ppt>2,2/22/9 TOX12C Iong2* 71 84 022499084 Tox 120, RBL02229-50ppb-2,2/22/9 TOX12C long2 72 8 5 022499085 Tox 120, RBL02229-100ppb-2,2/22/ TOX12C long2 73 86 022499086 Tox 120, RBL02229-250ppb-2,2/22/ TOX12C fong2 74 87 02249987 Tox 120, RBL02229-500ppb-2,2/22/ TOX12C long2 75 88 022499088 Tox 120, RBL02229-750ppb-2,2/22/ TOX12C long2 76 89 022499089 Tox 120, RBL02229-1000ppb-2,2/22 TOX12C long2 77 10 Analyte 10 QC ' 10 Analyte 10 Analyte 10 Analyte 10 Analyte 10 Analyte 10 Analyte 10 QC 10 Analyte 10 Analyte 10 Analyte 10 Analyte 10 QC 10 Analyte . 10 Analyte 10 Analyte 1 10 Analyte 10 Analyte 10 Analyte 10. Analyte 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 000550 FACT: DATA REVIEW SUMMARY FORM Date: c & f c f t f o Analyst FACT StudyNumber fD)C \ 2 0 Matrix IZ Jru Tune Points Dilutions? [Jo Analyte 1: Pfc> Acceptable LinearRange: LOQ for this data set Re-evaluatedfor differentrange? A) Analyte 2: Acceptable Tintar Range: Clot c *a 5 T ^ WfWCor^rs LOO fcr this data set ` t --- ^ Re-evaluated for different range? Analyte 3: roAA Acceptable LinearRnmw: L O Q fix(fatadataset: Re-evaluatedfor different range? l\b Analyte 4: .513, Acceptable Linear Rang e : /^ 0 ~~ / , <Dfaoppb> LOQ fortius data set /. = o Re-evaluated for.differentrange? Analyte 5: Acceptable Linear Rang e : /O -- ' ^ 5 0 pp3o LOQ for this data set b Re-evaluatedfor diffiarentrange? Analyte 6: Acceptable LinearRange: LOQ for this data set Re-evaluated for differentrange? Analyte 7: Acceptable Linear Range: LOQ for tins data set Re-evaluated ft rent range? 000551 BESTCOPYAVMUBtE Quantity Compound Summary Beport TGX-120 lUt Liver Cample Lint: C: \MASSbTlGC\rACT-l.*no\SeleDl\032499a Last modified: Wed Her 10 09:21:99 1999 Method: C:\HA8SLraX\rACT-l.rx0\MetfeOa\O22499a test modified: Tue Mar 09 13:93:43 1999 Job Code: Printed: Wed Mar 10 09:43:96 1999 >*ff1 Compound 1 roc Mama Saaplaliat Text Type Ctd Cone XT Area Si.. n a p e %Sev 1 022499001 *MeOH Blank Analyte 7.991 131 1 0.00 MM 2 022499002 3 022499003 4022499004 9 022499009 6 022499006 7 022499007 t 022499009 KtfOB Blank Tox 120 K B L Q 2 2 2 9 -H 2 0 Blk-1, 2/22/99 Tox 120, XBL02229-RBLivarBik-l.2/22/99 T ox 120. *BL02229-Sppb-1, 2/22/99 Tox 120. RBL02229-10ppb-l. 2/22/99 T o x 120. *BL02229-2Sppb-l, 2/22/99 Tox 120. BBL02229-S0ppb-1, 2/22/99 Analyte Analyte Analyte Standard Standard Standard Standard 5.99 12.00 29.90 59.90 7.941 .035` 7.960 7.992 7.991 7.986 91 418 961 642 1002 1612 ' 0.00 MM 5.18 HI 28.41 MMX 14.74 MMX 30.18 MM 56.29 MM 374 231 -6 9 022499009 Tox 120. K3L02229-100ppb-l. 2/22/99 10 022499010 T ox 120. XBL02229-250ppb-l. 2/22/99 11 022499011 Tox 120. RBL02229-500ppb-l. 2/22/99 . Standard Standard Standard 120.00 299.00 599.00 7.952 7.922 7.923 2898 7377 14301 111.40 MK 303.25 MM 599.79 MM -071 1 2 0 2 2 4 9 9 0 1 2 Tox 120, RBL02229-750ppb-l, 2/22/99 13 022499013 Tox 120. *BL02229-1000ppb-l, 2/22/99 Standard Standard S96.00 7.963. 1198.00 7.654 21841 27547 922.73 MM 1167.13 MM -33 14 022499014 MeOH Blank Analyte 15 022499015 Tox 120 DNO. 1457-C4, 2/22/99 Anelyte 7.954 3691 145.67 MM 16 022499016 Tox 120 DUO. 1467-G4, 2/22/99 Analyte 7.843 3012 116.29 MK 17 022499017 Tox 120 DNO. 1477-G4, 2/22/99 Analyte 7.852 2429 91.32 bb II 022499018 Tox 120 DNO. 1487-G4. 2/22/99 Analyte 7.766 ; 3388 132.39 MM 19 022499019 Tox 120 DNO. 1497-G4, 2/22/99 Anelyte 20 022499020 Tox 120, BBL02229-250ppb-CCU, 2/22/99 QC 7.822 299.00 7.854 2735 6536 104.39 MK 267.21 bb 21 022499021 MeOH Blank * ' Anelyte 22 022499022 T o x 120 10. 1507-G4, 2/22/99 Analyte 7.958 2709 103.27 MM 23 022499023 Tox 120 DNO. 1S17-G4, 2/22/99 Anelyte 7.797 3855 152.38 MM 2402 2 4 9 9 0 2 4 Tox 120 DNO. 1527-G4, 2/22/99 Analyte 7.863 2880 110.60 MK 25 022499025 Tox 120 DNO. 1S37-G4, 2/22/99 Anelyte 7.859 2305 77.44 MK 26 022499026 Tox 120 DNO. 1S47-G4. 2 /2 2 /9 9 Anelyte 7.829 3459 135.41 MK 2 7 0 2 2 4 9 9 0 2 7 Tox 120, RBL02229-250ppb-CC12, 2/22/99 QC 299.00. 7.BS7 587S( 238.88 KM 28 022499028 MeOH Blank Analyte 29 022499029 T a x 1 2 0 DNO. 1557-G4, 2/22/99 30 022499030 To* 120 DNO. 1577-G4, 2/22/99 Analyte Analyte 7.927 7.860 1975 4075 71.84 MM 161.80 MK 31 022499031 Tox 120 DNO. 158r>C4. 2 /2 2 /9 9 Anelyte 7.840 2570 97.34 MK 32 022499032 Tox 120 DNO. 1597-G4, 2/22/99 Anelyte 33 022499033 To x 120, RBL02229-250ppb-CClJ, 2 /2 2 / 9 9 Q C 7.856 299.00 7.569 4069 6615 161.56 MM 270.57 MK 34 022499034 MeOH Blank Analyte 35 022499035 Tox 120 DNO. 1617-G5, 2/22/99 Analyte 7.926 2634 100.10 MM 36 022499036 Tox 120 DNO. 1627-G5, 2/22/99 Analyte 7.846 1826 65.48 KM 37 022499037 Tox 120 DNO. 1637-G5, 2/22/99 Analyte 7.858 2079 76.32 KM 38 022499038 Tox 120 DNO. 164r-GS, 2/22/99 Analyte 7.665 3031 117.09 bb 39 022499039 Tox 120 DNO. 1657-05, 2/22/99 Anelyte 7.868 2013 73.46 MM 40 022499040 Tox 120. RBLO2229-250ppb-CCU. 2/22/99 QC 299.00 .7.836 6827 279.66 MM 41 022499041 MeOH Blank Analyte 42 022499042 TOx 120 DNO. 166r-GS, 2/22/99 43 022499043 Tox 120 DNO. 1677-05, 2/22/99 Analyte Analyte 7.937 7.869 2015 3075 73.56 MK 118.98 MK 44 022499044 Tox 120 DNO. 1687-05. 2/22/99 Anelyte 7.843 2398 89.96 IK 45 02249904S Tox 120 DNO. 1697-05, 2/22/99 Analyte 7.813 1835 65.85 MM 46 022499046 Tox 120 DNO. 1707-65 2/22/99 Analyte 7.858 1771 63.13 MK 47 022499047 Tox 120, RBL02229-250ppb-CC13, 2/22/99 Q C 299.00 7.838 7326 301.06 MK 48 022499048 MeOH Blank 49 022499049 Tox 120 DNO. 1717-65 2/22/99 Analyte Anelyte 7.947 1287 42.37 MM 50 022499050 Tox 120 DNO. 1737-05 2/22/99 Anelyte 7.825 1611 56.26 M K 51 022499051 Tox 120 DNO. 1747-65 2/22/99 Analyte 7.868 1421 48.15 MK 52 022499052 Tax 120 DNO. 1757-G5 2/22/99 Analyte 7.854 3019 116.58 MK 53 022499053 Tox 120 DNO. 1777-06 2/22/99 54 022499054 Tox 120, R8L02229-250ppb-CC16, 2/22/99 55 022499055. MeOH Bleak ' 56 022499056 Tox 120 pNQ. 1787-66 2/22/99 Anelyte QC Anelyte Analyte 299.00 7.750 7.861 7.869 7.921 2815804 8723 672 2500912 120593.. MM 360.87 MK 16.03 MK 107105.. MK \21 57 022499057 Tox 120 DNO. 1797-06 2/22/99 Analyte 7.849 2888958 123726. MK 58 022499058 Tox 120 DNO. 1807-66 2/22/99 Anelyte 7.856 2768001 119402.. MK 59 022499059 60 022499060 61 022499061 62 022499062 63 022499063 64 022499064 65 02249906S 66 022499066 67 022499067 68 022499068 69 022499069 70 022499070 Tox 120 DNO. 1817-06 2/22/99 Tox 120 DNO. 1827-06 2/22/99 Tox 120, RBL02229-250ppb-CC17, 2/22/99 MeOH Blank Tox 120 DNO. 1837-06 2/22/99 Tox 120 DNO. .1847-66 2/22/99 Tox 120 DNO. 1957-06 2/22/99 Tox 120 DNO. 1867-G6 2/22/99 Tox 120 DNO. 1877-66 2/22/99 T o x 120, RBL02229-230ppb-CC16. 2/22/99 MeOH Blank T ox 120 DNO. 189P-66 2/22/99 Anelyte Analyte QC Analyte Anelyte Anelyte Anelyte Analyte Anelyte QC Analyte Anelyte 299.00 299.00 7.752 7.576 7.854 7.927 7.931 7.853 7.653 7.849 7.861 7.861 7.931 7.937 3070609 2923061 10935 1317 2658942 2786810 2179533 2500338 2181490 9312 1129 1727B55 131506.. MK . 125187.'. M K I,n 455.64 H K 1 43.65 MM 1 113874.. HK 1 119351.. MK 1 93340.52 MK 1 107081.. MK 1 93424.33 MK 1 386.12 MK 1 35.60 MK 1 73994.38 MK 52 29 71 022499071 Tox 120 DNO. 1907-66 2/22/99 Analyte 7.862 2127694 1 91120.17 KK 72 022499072 T ox 120 DNO. 1917-G6 2/22/99 73 022499073 Tex 120, BBL02229-250ppb-CCl, 2/22/99 Analyte QC 7.788 299.00 7.871 2156366 10156 2 92348.31 MK 1 422.36 MK 41 74 022499074 MeOH Blank Analyte 7.867 1526 52.63 MK 75 022499075 Tox 120, 1107-Ol-250ppb-MS, 2/22/99 Analyte 7.696 13377 560.22 bb 76 022499076 T ox 120, 1107-61-250ppb-MSD, 2/22/99 Anelyte 7.782 15270 641.32 bb 77 022499077 T o x 120, HBL02229-250ppb-CC2, 2 /2 2 / 9 9 Analyte 76 022499078 MeOH Blank Analyte 7.848 7.947 5786 418 235.07 KM 5.17 MM 79 022499079 TOX 120, BBL02229-K20 Blk-2, 2/22/99 Anelyte 7.918 366 3.01 bb 80 022499080 Tox 120, BBL02229-XSUverBlk-l. 2/22/99 Anelyte 81 022499081 Tox 120, RBLQ2229-5ppb-2, 2/22/99 Standard 7.990 5.99 7.881 416 603 5.10 bb 13.08 Mia 118 82 022499082 83 022499083 84 022499084 85 022499085 86 022499086 87 022499087 88 022499088 89 022499089 T o x 120, RBL02229-10ppb-2, 2/22/99 T ox 120,. B3L02229-25ppb-2, 2/22/99 Tox 120, JtBL02229-50ppb-2. 2/22/99 T ox 120, RBL02229-100ppb-2. 2/22/99 Tox 120, RBL02229-250ppb-2. 2/22/99 Tox 120, KBL02229-500ppb-2, 2/22/99 T ox 120, R8L02229-750ppb-2. 2/22/99 T ox 120, BBL02229-1000ppb-2, 2/22/99 Standard 12.00 7.912 Standard 29.90 7.884 Standard 59.90 7.899 Standard 120.00 7.852 Standard 299.00 7.869 Standard 599.00 7.868 Standard698.00 . 7.665 Standard 1198.00 7.866 636 1180 1924 3319 7281 13610 20328 29544 14.50 bbX 37.81 MK 69.67 MK 129.40 HK 399.12 MK 570.21 MM 857.94 MM 1252.66 KM 21 26 16 0 -5 -45 VvlDOO Ytllbik O* (lb io* U LM S o u p 0 2 0 1 9 9 : Q u a n t i t a t e d o n 0 3 / 0 9 / 9 9 a n d p r i n t e d o n 0 3 / 1 0 / 9 9 b y DKB 000552 t i! 3^ :* 1 *i 43 ^ * oS 3 o 33 S S S j i l i S S 5 3 5 S S i S S3S25S3S33 33SSgS353 S8SSS5 r i ooo 5M 313 n-- o e 3 riH H H H H f4 H H H 3 3 53sssHs|=s SS55Ss Sas jj' '533SS55S SaiS Sis s 3 SSSSSSSSS s3 "ggssi i i i "5 -ts Rr Ci? s aaaaaaaaaaaaaaasssaa aaaaaa as s aa3383s33s3sas3ssasa sssapi ss IilSIs`!5 .....................\...i...i..y....i...-...m.... H i m s"a H H H H H H H H rtH H H H H riH H H H flH HrtrtrtrtH H H a s 3 p 5 | l | P | 5 3 5 1 | U s i l i II a aaa a asa s i H HHH oo^hAWonH O O <0 H I t H I H HH I II It aaaaaaaaa sssssssss "^'ssii HHHHHHHHH CO LO LO O O O l i S5S|i== SsSSssSSssSsss SSSss 33 33s33 i Si S 3 S 3 Sss s S 233333333 SS33SSSSS "sssass 3 Jt ?S3 !*? Ifl rS.43 jas :S53 !sss S 3 8 2 Si Iririririririri-' a sj* ! m SSi s! iliil ii il il il1 ili! i S S 5 3 S 3 3 3 'S 3 S S S 3 * 8 3 3 3 3 3 a 3S3^^^^ i!HI I s iss: l 1 i i i i l i i i i i i i i i i i i i i i i i i i i i i i i i i l i i i i i i i l i i i l i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i i s i i i i i i i i i i i i i i -- 33333as333saaaassR5saaaasasaaa333333S533gsaasssRSss3S332sc3sga{:aapsa2asss3ssssss TrT] 1 S U * oo-ooooooooooosoooooooooooggggogoog^ iiiiilliiiiiilil: il:"s:ss m if im iM m iffM M fK m m H H fm m fm m m im iM M fm E m m ifm ffK ffffH m iiii, sggSSsrS :5SgSSSSSSSSSS?&feSkgSiSSgSSSS! & e r ^ s i i r i s i lr 8'ssii i m ^h i i i i i ^ r 8g i i i ! i ; i i i i i ; i i s i E ; i i i i i m I il UliII Iil i iilllfi!mm m m ss :ssS is i s i ' s issi jfrr^l isS |ff ?! l-t s5 (M%- MHI? M OA *m ri ai il! SSS CS 89 crsr il iI SsssSssb,. skgkkssks % P S5HSa S s 4 sHs i Ma eo M B S. s j S Mt1a0 oo M1<00 oo M00 . ao M00 M1100 OO OO M1100 OO isSsSsKB. sssssssss S g I J *4 j Ni <4 J 4<4<4<44444 WHH 4OM0 HHJ bu HHH HeH SSSsSsss S Pir-*$r = m m - s22`5 uwIM 0oOkB. (MMM HMI 01 H 0toail M4100 004B10 S iS lIE E r ! r :* p s; 1 11 1 11 1 IsssHss m4HwMoAOOOMiuO* HHH H H / SES g " S 8 BH J woM o10\ b H OMJ wM H MHM M4 H 1MM0 b HH MM Ws OO oM H IMSHI HHHHHHHH SsSsSbs. b s b c b : O? 5 P i l M 5ss sss g - g g 3 S s S 5 S H M gg mB fC - f^c W1OI-IMMM1MIHHMO s1 MM1 MUi 4wH1 Hf1l HHi MH we1 B1 H1HHfcWOMVO0i1 i o c> O ^ K? O r i- S "* - - S ? &P - ou> O :*So ' loup 0301991 Quantitatad on 03/09/99 ani printad ob 03/10/99 by S M |g ig ssg i3 sisessgss|eesesssssssssssseissssssgsss3ssssssss :tt g3ggr2igIf282fggIV -gffSV ffgK fgV V K fggf|fV V gffB ffgV fgggffV gIggH gfV gfgV H l mmn lmBisisSkSs *** m u m u 3 m i * m t* ama s SSSs s s k ,. sssssssgs s s s s M SSSSpSSB.. sSaaa Bsasss Sss S 5 H M*4> H(MB s H sa *aCB . mwH SssSa 111111 HHH H H 'r H H H HH H H HHHHH iSssHs o o WN(MMA>a^it>t sm ss o cn HA1MU1U1WM cn cn SSS S skb b MB S CBi 5 2 g s G10 UO<n M1J0 w0 Ul b ggg t) .a- as tM b s b 0H1 MMO 001 g g ?. g 09 HMi 110 0H11 sSss ssass ggggg (a*ABH19H0CHiB P S g 11 a ! f o O Quantity Cenpousd S u a n r y A.port TCX-130 lUt Ll-nr O l a Li.t: C i M O a s t a \ > i*CI-l..MO\lulaoS\oa3>a tua aodifiad: Mad Kar 10 03:21:55 1 M Mathod: C:\HMSbnB\rjkCZ-l.MO\MatllOB\033493a Laat nadifiad: Tua Max 0* U : 5 1 : U 191) Bob Coda: \ Tintad: Mad Mar 10 09:43:30 1939 Ccnpouad Si K613 Mom ' t a p U U s f i Taxt 1 022499001 KaOH Blank 2 022499002 KaOH Blank Typa Analyta Analyta Std Cena ms 3 022499003 Tox 120, RBL02229-H20 Blk-1, 2/22/99 Analyta 4 022499004 S 022499003 6 02249900$ 7 022499007 8 022499008 9 022499009 10 022499010 1 1 022499011 12 022499012 13 022499013 T o x 120, XBU>2229~RBLivexftlk~l, 2/22/99 Tox 120, BBL02229-Sppb-1, 2/22/99 T o x 120, JtBL02229-10ppb-l. 2 / 2 2 / 9 9 To x 120, B8L02229-2Sppb-l. 2/22/99 Tox 120, RBL02229-50ppb-l, 2/22/99 Tox 120, *BL02229-100ppb-l, 2/22/99 To x 120, BBL02229-2S0ppb-l, 2/22/99 Tox 120, *BL02229-S00ppb-1, 2/22/99 Tox 120, BBL02229-7S0ppb-l, 2/22/99 * T o x 120, XBL02229-1000ppb-l, 2 / 2 2 / 9 9 Analyta Standard Standard Standard Standard Standard Standard Standard Standard Standard 5.99 12 .0 0 29.90 59.90 120.00 299.00 599.00 898.00 1198.00 9.373 9.374 9.398 9.380 9.345 9.347 9.289 9.280 ] 14 033499014 15 033499013 1 033499010 KaOH Blank Tox 130 OHO. 14SF-64, 3/33/99 Tox 120 DUO. 146,-64. 2/23/99 Aanlyt. Bnalyta taalyta 17 022499017 Tox 130 OHO. 147V-04, 2/22/99 Analyta 18 022499018 Tox 130 OHO. 1489-04, 2/22/99 Analyta ' 19 022499019 Tox 120 OHO. 1499-04, 3/22/99 Analyta 20 022499020 T o x 130, UL02229-250ppb-CCll, 2/23/99 QC 299.00 9.280 21 032499021 KaOH Blank Analyta 32 022499023 Tox 110 OHO. 1509-04, 2/22/99 Analyta 21 022499023 Tox 120 DMO. 1319-04, 2/22/99 Analyta 24 022499024 Tox 120 DHO. 1S29-G4, 2/22/99 Analyta 23 022499025 Tox 120 SHO. 1339-04, 2/22/99 Analyta 28 022499026 Tox 120 DHO. 1549-04 , 2/22/99 Analyta 27 022499027 T o x 120, ABL02229-250ppb-CC12 , 2/23/99 QC 299.00 9.374 28 022499028 KaOH Blank Analyta 29 022499029 T a x 120 UNO. 1559-04. 2/22/99 Analyta 30 022499030 Tox 120 DHO. 1579-04 , 2/22/99 Analyta 31 022499031 T o x 120 DHO. 1589-04, 2/22/99 Analyta 32 022499032 T o x 120 DHO. 1599-04, 2/22/99 Analyta 33 022499033 T o x 120, ABL02229-250pk-CC13, 2/22/99 QC 299.00 9.279 34 032499034 KaOH Blank Analyta 33 022499035 T o x 120 DMO. 1519-05, 2/22/99 Analyta 35 022499038 T o x 120 DHO. 1529-05. 2/22/99 Analyta 37 022499037 Tox 120 DHO. 153r-05 , 2 /2 2 /9 9 Analyta 38 022499038 T o x 120 DHO. 184r-OS, 2/22/99 Analyta. 39 022499039 T o x 120 DHO. 1559-05, 2/22/99 Analyta 40 022499040 T o x 120, RBL02229-25Oppb-CCl4, 2/22/99 QC 299.00 9.262 41 022499041 KaOH Blank Analyta 42 022499042 T o x 120' DHO. 1689-05, 2/22/99 Analyta 43 022499043 T a x 120 DHO. 1679-G5, 2/32/99 Analyta 44 022499044 Tox 120 DMO. 1689-05. 2/22/99 Analyta 45 022499045 Tox 120 DHO. 169r-OS. 2/22/99 Analyta 46 022499046 Tox 120 DHO. 1709-GS 2/22/99 Analyta 47 022499047 Tox 120. BBL02229-250ppb-CC15, 2/22/99 QC 399.00 9.262 48 022499048 KaOH Blank Analyta 49 022499049 Tox 120 DHO. 1719-G5 2/22/99 Analyta 50 032499050 Tox 120 OHO. 1739-CS 2/22/99 Analyta 51 022499051 TOX 120 DHO. 1747-05 2/22/99 Analyta J 32 022499052 53 022499053 54 022499054 TOX 120 DHO. 1757-65 3/22/99 Tox 120 DHO. 1777-G6 2/32/99 Tox 120, RaL02229-250ppfa-CC16. 2 /2 2 /9 9 Analyta Analyta QC 299.00 9.287 55 022499055 MoOH Blank Analyta 56 022499056 'Tox 120 DHO. 1787-66 2/22/99 Analyta 57 022499057 Tox 120 DHO. 1797-66 2/22/99 Analyta 58 022499058 Tox 120 DMO. 1807-66 2/22/99 Analyta 59 023499059 Tox 130 OHO. 1817-66 2/32/99 Analyta 60 022499060 Tox 120 DHO. 1627-66 2/22/99 Analyta 61 022499061 T o x 120, B8D02229-250ppb-CC17, 3/23/99 QC 299.00 9.277 62 022499062 KaOH Blank Analyta 63 023499063 T ox 120 DHO. 1837-66 2/22/99 Analyta 64 022499064 Tox 120 DHO. 1847-66 2/22/99 Analyta 65 022499065 T ox 120 DHO. '1657-66 2/22/99 Analyta 66 022499066 T ox 120 DHO. 1667-06 2/22/99 Analyta 67 022499067 Tox 120 DMO. 1877-66 2/22/99 Analyta 68 022499068 T o x 120, Ut02239-3S0ppb-CC18, 2/22/99 QC 299.00 9.287 69 032499069 KaOH Blank Analyta 70 022499070 Tox 120 DMO. 1697-66 2/32/99 Analyta 71 022499071 TO X 130 DHO. 1907-66 2/22/99 Analyta 72 022499072 T ox *120 DHO. 1917-66 2/22/99 Analyta 73 022499073 T o x 120., HBL02229-250ppb-CCl. 2/22/99 QC 299.00 9.289 74 022499074 KaOH Blank Analyta 75 022499075 T o x 120, 110,-61-250ppb-MS. 2/22/99 Analyta 9.367 76 022499076 T o x 120, 110T-61-230ppb-KSD, 2/22/99 Analyta 9.295 77 022499077 T OX 120, MBL02229-250ppb-CC2, 2/33/99 Analyta 9.253 78 022499078 KaOH Blank Analyta 79 022499079 T ox 120, R B U 2 2 2 9 - K 2 0 Blk-3, 2/22/99 Analyta 60 022499080 T o x 120. RBL02229-RBUvacBlk-l, 2/22/99 Analyta 81 022499081 T ox 120. MBL02229-5ppb-2, 2/22/99 82 022499082 T ox 120, RBLQ2229-10ppb-2, 2/22/99 Standard Standard 5.99 12.00 83 022499083- Tox 120, XBD02229-2Sppb-2, 2/22/99 Standard 29.90 9.297 84 022499084 T o x 120, HBL02229-50ppb-2, 2/22/99 Standard 59.90 9.311 85 022499085 T o x 120, BBb02229-100ppb-2, 2/22/99 Standard 120.00 9.278 66 022499086 T o x 120, MBL02229-250;b-3, 2/22/99 87 022499087 T o x 120, RAL02229-500ppb-2, 2/22/99 - Standard Standard 299.00 9.295 599.00 9.294 aa 022499088 To x 120, RBl02223-750ppb-2. 2/22/99 Standard 898.00 9.293 89 022499089 T ox 120. RBL02229-1000ppb-2, 2/22/99 Standard 1198.00 9.294 lo u p 020109: Q u u t l t i t s d p a 0 3 /0 9 /9 9 pad p r in te d o a 0 3 /1 0 /9 9 b y drb I A n a Di Cons. lo Mo o t 44 89 148 281 $10 116$ 1788 2127 1 8.41 MM 1 32.10 bb 1 63.32 MM 1 133.38 bb 1 307.64 bb . 1 602.07 bbX 1 930.80 bbX 1 1110.50 bbX -30 7 6 11 3 1 4 -7 460 1 239.14 bb 459 1 227.79 bb 561 1 282.01 bb 571 1 287.06 bb 634 . 1 320.22 bb 584 1 293.99 b b 578 1 290.74 bb 489 1 243.59 bb 307 1 253.42 bb 446 1 220.79 MM 466 1 231.31 MM 62 142 260 566 1158 1610 2343 1 17.83 MM 1 59.88 MX 1 122.65 MX 1 284.38 MM 1 397.74 bbX 1 836.67 MMX 1 1224.94 MMX 0-40 2 -S0 -7 2 00055S S* 3 O')] guaaetfy Cnpoiusd tv m a a x y a p o n TOX-13Q lut Livar Sanpla Piati C:\WUaL-nJX\7ACT-l.ano\IanBlaDB\02219S* La. laodlfladi N ad Mac 10 OSiSXtSS 1191 Katbod: Ct\MXSSLmX\nCT-l.MO\MatllBB\0224m Laat aodlCladi Tua Har OS 1 3 : 3 1 : 0 U S 9 Job Codai Sx lat ad ' M a d Mar 10 0 9 i O i 5 1S9S COoponad St If 1 Mum Saxplaliat Text Typa Std Cone 1 022499001 KcOH Blank Analyta 2 022499002 MaOH Blank Analyta 2 022499003 T o x 120 BBL02229-X2O Blk-1. 2/22/99 Analyte 4 022499004 T O x 120 ftBL02229-RBLiverBlk-l, 2/22/99 Analyta S 022499005 Tox 120 XBL02229-5ppb-l 2/22/99 6 022499006 T ox 120 RB102229-10ppb-l, 2/22/99 Standard Standard 494.00 494.00 7 022499007 9 022499008 9 022499009 10 022499010 Tox 120 KBt02229-2Sppb-l, 2/22/99 Tox 120 BBL02229-50ppb-l, 2/22/99 Tox 120 XBL02229-100ppb-l, 2/22/99 T o x 120 BBL02229-250ppb-l, 2/22/99 Standard Standard Standard Standard 494.00 494.00 494.00 494.00 11 022499011 Tox 120,BBL02229-500ppb-l, 2/22/99 12 022499012 Tox 120 HBL02229-750ppb-l, 2/22/95 Standard Standard 494.00 494.00 13 022499013 To x 120 BBL02229-1000ppb-l, 2/22/99 Standard 494.00 14 022499014 MaOH Blank Analyta IS 022499015 T O X 120 DNO. 1457-434, 2/22/99 Analyta 16 022499016 T o x 120 DUO. 1467-04 2/22/99 Analyta 17 022499017 TOX 120 DNO. 1477-64, 2/22/99 Analyta 18 022499018 Tox 120 DNO. 1467-G4, 2/22/99 Analyte 19 022499019 Tox 120 DNO. 1497-04. 2/22/99 20 022499020 To x 120, U L 0 2 2 2 9 - 2 5 0 p p b - C C U # 2/22/99 Analyta QC 494.00 21 022499021 MaOH Blank Analyta 22 022499022 T O X 120 DMO. 1907-04, 2/22/99 Analyta 23 022499023 TOX 120 DNO. 1517-04, 2/22/99 Analyta 24 022499024 Tox 120 ONO. 1527-C4, 2/22/99 Analyta 25 02249902S Tox 120 DNO. 1537-G4 2/22/99 Analyta 26 022499026 Tox 120 DNO. 1547-64, 2/22/99 Analyta 27 022499027 Tox 120, BBL02229-259ppb-GC12, 2/22/99 oc 494.00 26 022499028 MaOH Blank Analyta 29 022499029 T o x 120 ONO. 1557-C4, 2/22/99 Analyta 30 022499030 T9X 120 DNO. 1577-64, 2/22/99 Analyta 31 022499031 Tox 120 DNO. 1587-64, 2/22/99 Analyta 32 022499032 Tox 120 DNO. 1597-64. 2/22/99 Analyta 33 022499033 T ox 120, kBL02229-250ppb-CC13, 2/22/99 QC 494.00 34 022499034 MaOH Blank Analyta 35 022499035 T O X 120 DNO. 1617-05, 2/22/99 Analyta 36 022499036 Tox 120 ONO. 1627-QS, 2/22/99 Analyta 37 022499037 Tox 120 DNO. 1637-65, 2/22/99 Analyta 38 022499038 T ox 120 DNO. 1647-05, 2/22/99 Analyta 39 022499039 Tox 120 DNO. 165r-OS, 2/22/99 Analyta 40 022499040 T o x 120, HBL02229-250ppb-CC14, 2/22/99 QC 494.00 41 022499041 MaOH Blank Analyte 42 022499042 Tox 120 DNO. 1667-05, 2/22/99 Analyte 43 022499043 Tox 120 DNO. 1677-05, 2/22/99 Analyta 44 022499044 Tox 120 DNO. 1687-05. 2/22/99 Analyta 45 022499015 Tox 120 DNO. 1697-05, 2/22/99 Analyta . 46 022499046 T ox 120 DNO. 1707-05 2/22/99 Analyta 47 022499047 T o x 120, XBL02229-2S0ppb-CC15, 2/22/99 QC `494.00 48 022499048 MaOH Blank Analyta 49 022499049 Tox 120 DNO. 1717-GS 2/22/99 Analyta SO 022499050 Tox 120 DNO. 1737-05 2/22/99 Analyta SI 022499051 T o x 120 DNO. 1747-05 2 /2 2 /9 9 Analyta S2 022499052 T o x 120 DNO. 1757-05 2/22/99 Analyte S3 022499053 Tox 120 DNO. 1777-06 2/22/99 Analyta 54 022499054 Tox 120, BBL02229-250ppb-CC16. 2/22/99 QC 494.00 55 022499055 MaOH Blank Analyta 56 022499056* T ox 120 DNO. 1787-06 2/22/99 Analyta 57 022499057 T o x 120 TOO. 1797-06 2/22/99 Analyta 58 022499058 Tox 120 DNO. 1807-08 2/22/99 Analyta 59 023499059 Tox 120 DNO* 1817-06 2/22/99 Analyta 60 022499060 T o x 120 DNO. 1827-66 2/22/99 Analyta 61 022499061 T ox 120, KBL02229-250ppb-CC17, 2/22/99 QC 494.00 62 022499062 MaOH Blank Analyta 63 022499063 T O x 120 DNO. 1837-06 2 / 2 2 / 9 9 Analyta 64 022499064 T o x 120 ONO. 1847-66 2/22/99 Analyta 65 022499065 TOX 120 DNO.*1857-06 2/22/99 Analyta 66 022499066 T ox 120 DNO. 186r-G6 2/22/99 Analyta 67 022499067 T ox 12 DNO. 1677-06 2/22/99 Analyta 68 022499068 T o x 120, R8Cs02229-250ppb-CC19. 2 / 2 2 / 9 9 QC 494.00 69 022499069 MaOH Blank Analyta 70 022499070 TOX 120 DNO. 1897-66 2/22/99 Analyta 71 022499071 T ox 120 ONO. 190P-G6 2/22/99 Analyta 72 022499072 T o N 120 DNO. 1917-66 2/22/99 Analyta 73 022499073 T ox 120, ftBlA2229-250ppb-CCl. 2/22/99 QC 494.00 74 022499074 MaOH Blank Analyta 75 02249907S T O X 120. 1107-61-250ppb-MS, 2 / 2 2 / 9 9 Analyta 76 022499076 T ox 120, 1107-Gl-250ppb-MSD, 2/22/99 Analyta 77 022499077 Tox 120, BBL02229-250ppb-CC2. 2/22/99 Analyta 78 022499078 MaOH Blank Analyta 79 022499079 T ox 120, R8L02229-H2O Blk-2, 2/22/99 Analyta 90 022499080 T ox 120, ftBL02229-RBLiverBlk-l. 2/22/99 Analyta 91 022499081 T ox 120, RBL02229-5ppb-2, 2/22/99 Standard 494.00 82 022499082 T ox 120, RBL02229-10ppb-2, 2/22/99 Standard 494.00 83 022499083 T ox 120, *BL02229-25ppb-2, 2/22/99 Standard 494.00 84 022499084 Tox 120, HBL02229-50ppb-2, 2/22/99 Standard 494.00 65 02249908S T OX 120, KBL02229-100ppb-2, 2/22/99 Standard 494.00 86 022499086 T ox 120, BBt02229-250ppb-2, 2/22/99 Standard 494.00 87 022499087 T ox 120, RBL02229-500ppb-2, 2/22/99 Standard 494.00 88 022499088 T o x 120, RBL02229-750ppb-2, 2/22/99 Standard 494.00 89 022499089 T ox 120, RBt02229-1000ppb-2, 2/22/99 Standard 494.00 Jtt 7.314 7.320 7.252 7.236 7.235 7.194 7.237 7.209 7.122 7.145 7.13S 7.237 7.136 7.050 7.049 7.116 7.138 7.163 7.082 7.062 7.142 7.031 7.060 7.212 7.142 7.130 7.054 7.072 7.209 7.131 7.144 7.063 7.160 7.119 7.223 7.068 7.130 7.106 7.057 7.124 7.231 7.112 7.151 7.138 7.035 7.145 7.211 7.134 7.059 7.037 7.035 7.141 7.131 7.142 7.137 7.135 7.143 7.145 7.137 7.068 7.080 6.996 7.152 7.066 7.050 7.208 7.197 7.169 7.122 7.093 7.105 7.136 7.068 7.066 7.064 7.064 Araa Dl Cone. Tlaga kDev 348 278 665 847 768 713 583 663 675 673 746 389 632 421 472 617 672 329 481 599 560 402 555 316 473 464 362 654 383 676 588 604 515 558 349 497 586 441 353 542 340 534 513 493 231 SIS 236 216 226 235 204 571 199 225 281 206 308 575 285 351 306 546 322 366 531 308 316 70 704 756 748 691 732 642 638 537 1 248.61 MM 1 198.55 bfa 1 474.76 MK 1 604.74 MK 1 548.31 bb 2 509.24 bb 1 416.56 bfa 1 473.22 bfa 1 482.12 MM 1 480.59 bb 1 532.80 bb -50 -60 -4 22 11 3 -16 -4 -2 -3 8 1 278.17 MM 1 451.67 bb 1 300.56 bb 1 336.95 bb 1 441.04 bb 1 480.18 bb -44 -9 -39 -32 -11 -3 1 235.15 bb -52 1 343.87 bb - .30 1 428.10 bb .-13 1 414.05 M K r 287.31 bb -16 -42 i 396.73 bb -20 i 225.86 MM i 337.66 MM i 331.42 MM 2 258.72 bb 1 466.87 bb -54 -32 -33 -48 -5 1 273.25 MK 1 482.50 bb .1 420.31 bb 1 431.38 bb 1 367.61 bb 1 398.50 bb -45 -2 -15 -13 -26 -19 1 249.01 bb 1 355.24 bb 1 418.91 MM 1 314.98 bb 1 252.29 MX 1 387.24 MM -50 -28 -15 -36 -49 -22 1 242.98 MM 1 381.17 fab 1 366.66 MM 1 352.10 MK 1 164;71 MX 1 367.80 bb -51 -23 -26 -29 -- 67 -26 1 168.62 bb 1 154.58 bb 1 161.28 M X 1 167.67 fab 1 146.02 bb K 407.90 bb i 142.43 bb i 1643.54 b b i 200.47 MK i 148.91 bb i 220.14 bb i 410.85 bb -66 -69 -- 67 -66 -70 -17 -71 -68 -59 -70 -55 -17 i 203.31 bb i 250.92 MK i 218.67 bfa i 389.67 bb i 229.80 bb i 261.34 bb i 379.16 bb i 219.86 MM i 226.93 XX i 478.13 XX i 902.64 bb i 940.16 bb i 533.98 bb i 493.58 bb i 523.07 MM i 458.22 bb i 455.91 bb i 313.25 MM -59 -49 -56 -21 -S3 -47 -23 -55 -54 -3 2 9 8 0 6 -7 --8 22 Soup 020ISS i Q u a n tlta ta d o a 0 1/0S /S S an d p d a t a d o a 0 3 /1 0 /9 9 b y m 000557 Vasa Q u a n tify C a lib ra tio n te p o rt TCX-120 a t l i r a * Calibration: C i M I U I U I B \ n c i - t . n o \ c u n n M I ] U a Laat laodifiad: M a d Max 10 0 9 : : 03 1999 rintad: Mad Max 10 00:44:01 1000 *aga X lo u p 030100: Q u a n tita ta d o n 0 3 /0 0 /0 0 an d p x la ta d on 0 3 /1 0 /0 0 b y su a 000558 Oua n e l i y C a l i b r a t i o n B a p o rt TOX- 1 2 0 l u e U v a r calibration c>\MaMian\ric>-l.PM\curraBS\0324*a taat nodifladi ad Mar 10 Mi43iOS I J Paint ads W a d Mar IS OS U i 01 ISSS c u p 0 2 0 1 S S I Q o a a t l t a t a d o n O S /O S /S S a n d p r l n t a d o n 0 3 / 1 0 / S S t r y UHM 000559 Quaatlfy Calibrati apere tax-iao aae U t u Calibrati: c:\nanuicc\racf-l.no\CaraaDa\0331Ma Late acdiflad: ad Kar 10 03:43:03 ISO* relatad: ad Mar 10 03:44:01 1333 Vaga 3 lo u p 030133: Q u aaeltaead o a 0 3 /0 3 /3 3 a a d p r la ta d o a 0 3 /1 0 /3 3 far S ta 000560 Quantify c alibration Jtapoxe OX-120 xae b i-m r Calibration! Ci \ M M M N X \ n - l .I*O\CuraaIJ\03241a M a t aodifiad: M Max 10 01:43:0s loss yrintad: a d Max 10 Ofi44i01 Ifff ) *0 4 *oup 0301591 Q u a n tita ta d e n 0 3 /0 1 /1 an d p r in ta d a n 0 1 /1 0 /9 1 b y SM 000561 Q u a n tity C a lib ra tio n to s e n TC X -120 afe U w a r Calibration: Cs\NU*Z<l\ncS<l.ntO\cuzvan\>33Mla beat aoditladi tod Mar IS 05]43:OS 1S5J rintad: ad Mar 1 05:44:01 1 Soup 0 2 0 1 9 h Cuanti catad o n 0 3 / 0 9 / 9 9 aad printed e n 0 3 / 1 0 / 9 9 D y D U 000562 Quantify Calibration M p o r t W3X-120 tat Litar Calibration! C:\XUlLrax\racT-l.nO\CurvaBa\022199a Last nodlflad) Wad H u 10 09>t2:OS ISOS Tintad! Wad War 10 Ots U i O l 1 lo u p 0201991 Q u a n tita ta d on 0 3 /0 9 /9 9 an d p r ln ta d o n 0 3 /1 0 /9 9 b y r a t 000563 Mmtbcd p e rt Hathed f i l a t Laat aed lfiad i Coapoundt Ci \XASSLYIfXNTXCT-l.rRO\KathDB\022499a.ia31J f r i Pab 3 1 0 i3 0 il9 139 li PPOS P r in t< d l____________ t u . K r 0 1 3 .3 3 ,0 1 1993 Compound S a M t Internal Sf>i Quantify Trace* Cone, of Standards* Vsar RP Valttai Daar Peak Paccori Xnt.gr.t. Window Pacteri PPOS (Nona) TIC Cone. A 1.000000, Disabled 1.000000 a.ooo Ratancion Tina (mina) i Ralatlva R.caution Tiaai Tint. Window (min.) i Task Saloctiom 1.03, tnablad 0.000. Diaablad 1.030 Dearest Aeaponse Types Responses Ixtexnal Areas Polynomial Type* Point of Origin* Pit Weightings Axis Transformation* Linear Bxeliade XOne Dnltai Peak-to-peak amplitudes iss Smoothing* Window size (scans)* Number of smooths* Smoothing methods Disabled 1 2 Join valley threshold* Seduce peek tailings Seize baseline maximum* 30.00 70.00 4.00 Draw vertical threshold* Detect shoulderst Shoulder threshold* 10.00 Diublad 10.00 Relative heights Absolute heights Relative areas. Absolute area* 30.00, Enabled , 0.00p Disabled 3.00* Inabled .0.00. Disabled fagt j S o U p 0 3 .0 1 ^ L A C 0 3 _________________________________ # .! . ^ ' * 000S64 M ethod R e p o rt M a thod filai Laat modified! Compound! printed! C: \MASSLYNX\rRCT-l.PRO\M.thEB\02H 9 9 a . m d b Tri T ab 26 10i3 0 i 39 1999 2i ?ras . Tua M a r 09 1 1 i2 2 i01 1999 Compound Nanai I n t a n a i Ra. 1 Quantify Tracal Cone, of Standards! Usar HP Valuei Usar Peak Paetori Integrata Window Pactor: WHS (Nna] TIC Cone. A 1.000000, Disabled 1.000000 2.000 Retention Tine (alna) t Relative Retention Tine Tine Window (nina) i Peak Selectioni .363, enabled 0.000, Disabled 1.117 Keenest Response types Responses Internal Arena Polynomial types Point of Origins Pit Weightings Axis TransCessation Linear Seclude Bone Bone Quitss Peak-to-paak aaplftude* Ih j i Window size (scans)i Dumber of smoothsi Smoothing method! 115 Disabled 1 2 Join valley threshold! * Reduce peak tailing Raise baseline maximum 30.00 70.00 4.00 Draw vertical thresholds Detect shoulders Shoulder thresholds 10.00 Disabled 10.00 Relative height! Absolute heights Relative areas Absolute areas 50.00 Knabled a 0 .00, Disabled 3.00, Knabled 0.00, Disabled Vaga 2 Soup m onv LAC n i l i l w 000565 M ethod R e p o rt Method f l l e i te a t M odified! Compound: Printed! C !\W A SSl\rA CT-l.PR 0\H ethI\022499e.edli P r l Teh 2S 10 00, 1 1999 3 *0** Tue Her OS 13i22i01 1999 Compound N u t t Internal M t . i Quantify Traeai. Cone, of Standardai Dear XT Value i Deer Teak Taetori Integrate Window Factor! nu . (Hone) TIC Cone. A 1 .000000, Diaahled 1.000000 2.000 Retention Time (mins) * Xelative Retention Timei Tin* Kladov (mine) Teak Selection! 7.490, Xneblad 0.000, Disabled 0.902 Meareat Xaeponae Typei lspout Polynomial Typei Point of Origin! Tit Weightingi Axle Trane formation i Xru elude gpim mime Units* Peak-to-peak aajplltudat 185 Smoothing* Window ni*o (scans)i number of smooths Smoothing method! . Disabled 1 2 Join valley threshold!' Reduce peak tailing! Raise baseline marine! 30.00 70.00 4.00 Drew vertical threshold Detect shoulders Shoulder threshold 10.00 Oiaabled 10.00 Xelative height Absolute height Xelative area* Absolute areas 50.00, Enabled , 0.00, Disabled 3.00 Enabled 0 .00 Disabled Soup dZqiM IAC 031Oik1 000566 Kathod f ll i L u c aodilled! Compound! Printed! C t\]U SS Z ,m rA C T -l.PliO U lehO a\023199a-*<U >. Fcl r.b 2 IO1IO1 1999 11 HSU Tut Mar 09 13i22OX 1999 Compound Hanoi Internal Ref.i Quantify Tracei Cone, of Standardes User AT Valuot User Peak Pactori Integrate Window Pactori X913 (HOno] TIC Cone A 1 .000000, Diaablod 1.000000 3.000 Retention T ine (nine) Relative Retention Tiaoi Tine Window (nine) i Peak Selection! B.S4S, Enabled 0.000, Disabled 0.730 nearest Response Typei Response! External Aroan Polynomial Typei Point of Oriffin i Pit Weighting! Axis Transformation' Linear Exclude Wona Kona Unite2 Peak-to-peak amplitude! * IBS Snoothinffi Window sire (scans) x unbar of smoothai Smoothing method i Diaablad -1 2 Join valley threshold! Reduce peak tailingi Raise baseline suximusu 30.00 70.00 .4.00 Draw vertical threshold! Detect shoulders! Shoulder threshold! 10.00 Disabled 10.00 Relative height! Absolute height! Relative area.t Absolute areat . 50.00, enabled , 0.00, Disabled 3.00, Rnabled . 0.00, Disabled Soup 020m LAC &blo4v\ j? . 000567 Method Repart Method filai Lest modified! Compound: printedi Ci \MASSLYNX\rACT-l. PHO\HsthDB\03J499e.mdb fri Tab It 10i30t39 199) Si MS 13 Tue Her 09 13i33i01 1999 Compound Marne Internal Ref.i Quantify Trace! Cone, of standardet Osar RP Value t User peek Vectors Integrate Window Vectori Mill (Monel TIC Cone. A 1.000000, Disabled 1.000000 3.000 Retention Time (mins) i Relative Retention Timet Time Window (mine) t Peak Selectiont 9.591, Rnefaled 0.000, Disabled 0.730 Nearest Response Type MSpOOMi Polynomial types Point of Origins pit Weightingi >xie Tramafexmatioat ^eternal Areas Trl BNCluda Rone Rone tJfcitsi Peafc-to-paafc anplitudst Smoothing! Window aixa (scene) t Number of smooths! Smoothing methods Join valley threshold! ' Reduce peek tailings Raise baseline mexinumi Draw vertical thrasholdi Datact shoulders* Shoulder thresholds Relative height! Absolute height! Relative areas. Absoluta areas 1RS* Disabled 1 3 30.00 70.00 4.00 10.00 Disabled 10.00 30.00, enabled 0.00, Disabled 3.00, Rnebled 0.00. Disabled 5duo oaom 1 ' '* . i a c ciIm Iw 000568 M ethod p o rt Method idle i Last nodifieds Compound t printedi C. \MASSL7HX\fACT-l. PRO\HethDB\023499a.sdb Pri eh It 10 s10-.19 1999 Si IS Tam H er 9 1 1:23.01 1999 Cenpound Hanses I n t e m e l Ref.s Quantity Trace> Cone, of Standardas Dear U Valuei Uaer Peak Pactozi Integrate Window factors 13 [Hone] TIC Coae. a 1.000900, Disabled 1.000000 2.000 Retention Time (mine) Relative Retention Times Tine Window (mine] s Peak Selections 7.410 enabled 0.000, Diaabled 0.990 Heareat Response Types Polynomial Types Point ot origins Pit Weightings Riaie Transformations Unear Kssclude Nona Unites Peak-to-peak asssplitssdes Smoothing s Window size (cans!s Humber of asnoothas Ssssoothing methods Diaabled .1 3 join alloy threshold: Radsice peak tailings Raima baseline manimums 30.01 70.01 4.00 D raw vesrtical thresholds Detect shoulderss Shoulder threshold: Relative heights Absolute heights Relative areas Absolute areas 10.00 Disabled 10.00 50.00, Haablad 0.00, Disabled 3.00, Snabled 0.00, Disabled SpUj) 0%cm U c Qilo'ilw 000569 M ADELINE 041098: FACT E quipm ent Log 98053 U A PAGE I Q uattro II, #6443E 1 DATE: 03/01/99 ANALYST: drb STUDY NUM BER TOX 120 M ATRIX: ra t liver DESCRIPTION: liver extr. dilutions ] FACT M ethod: _ Injection volume, 10 uL Cycle tim e: 16 m in. Electrode: Z-Spray_______ 1 MobUe Phase: (AM.O mM NH4CH3CQ2 . (B) MeOH_____________ TN-A- o r stadrd num ber (A) 99011-1-9_________ QB) TN-A-2384 ] Prepared (date/by): ` ' ( A) 2/12/99 m ee_________ " (B) 2/20/99 dib E x p ires: (A) 08/12/99___________ (B) 8/18/99_____________ ] Store at room tem p? (Yj o r N O th er_________________________ T G uard colum n: None________________ .__ P art number: na ________ L ot num ber: na_________________________ I A nalytical colum n: keystone betasil__________ i Size: 2 x 100mm__________ . T y p e:c l8 __________ Sphere size: Sum _____________ i t P art num ber: 105-701-2_______ L ot number: p8f!3 Serial number 118739a ] j A nalytical param eters: D rying gas (L/hr): 300 ESI nebulizing'gas (L/hr) 15 Sheath gas (L/hr) 0 - J LC Flow rate: 300 uL/m in. B ack pressure: 120 bar 3 H PL C solvent g rad ien t: long2ex J Time (min.-) 1) 0.00 %B 40 2) 8.5 90 I 3 1.1.0 4 )iy_ 51 12.5 I 6) 13.00 90 100 100 40 > . ' ] 000570 1 Tuning Method Report Method: C :\MASSLYNX\RATS. PRO\ACQUDB\PFOS Printed: Mon M a r 01 17:17:40 1999 . . M W _____ ( A L o r / i o l v Page 1 BESTCOPYAVAILABLE MS SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. Set Rdbk 3.00 45 5 0.2 150 250 3.00 -46 -4 153 251 Pressures Analyser Vacuum Gas Cell Rdbk 6.4e-5 5.3e-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier Set 15.0 15.0 2.0 ? 0.0 ' 5 650 MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set Rd 15.0 15.0 20 2.0 0.0 40 0 650 20 41 18 000571 S c a n n in g MaChod R e p o rt H athod: l a s t M odiriad: P rinted: C:\HhS9LYNX\RhTS.PR0\ACQUDB\TOX12QA Mon M ar 01 1 7 :1 6 :3 1990 Mon M ar 01 1 7 :1 7 :5 1 1999 , n iJ jJ iu S olvant B alay ( alna > i 0 .0 0 <s> rtM to u .. LAC runetion t 1 MM o ( 3 Mata P a i r s ESP- ) In ta r Channal Balay ( Saca ) i Span ( D altona ) t S t a r t T la a ( Mina ) : End T laa t Mina ) i Rapaata i Channal P arant D aughtar o .o a 0.00 0.00 13.50 1 D w sll (s.c a ) C e l l E n erg y <eV) Cons 1 399.00 80.00 0 .2 5 2 399.00 99.00 0.25 3 399.00 130.00 0.25 45 45 45 0 0 60 j ] r : 1 runetion S 3 MM o f 3 Maaa P a i r s ESP- 1 In ta r Channal Balay ( Saca ) i Span ( S altona ) : S t a r t T la a ( Mina ) t End T laa < Mina ) i Rapaata i Channal P arant O aughtar 0 .0 3 0 .0 0 0 .0 0 13.50 1 D w sll (Sees) ' c o li Energy (aT) 1 499.00 90.00 0 .2 5 2 499.00 99.00 0 .2 5 3 499.00 130.00 0.25 45 45 ' 45 Cons Cv | 60 60 60 Ponction : 3 MRM o f 3 Maaa P a i r s C ESP- ) In ta r Channal Balay ( Saca ) i Span ( D altona ) i S t a r t T laa ( Mina I I End T laa t Mina ) t Rapaata : Channal P aran t Daughtar 0.03 0 .0 0 0 .0 0 13.50 1 D w sll ISaca) C oli Energy taV) Cons 1 299.00 90.00 . 0.25 2 299.00 . 99.00 0.25 45 45 35 35 runetion : 4 MRM o f 3 M u s P a ir a < ESP- > I n ta r Channel Dalay ( Seen ) : Span ( D altone ) S t a r t T la a ( MIna ) 1 End T laa ( Hin ) t R apaata : Channal P arant Daughtar 0 .0 3 0 .0 0 0 .0 0 13.50 l D w sll {Saca) C o ll E nergy (eV) 1 413.00 119.00 0.25 2 413.00 199.00 0.25 3 413.00 219.00 0.25 30 20 30 Cons ( V > 15 15 15 J runetion < S MRM of 3 Maaa Paira ( ESP- I Zntsr Chsansl Dslsy ( Saca ) i 0.03 Span < Osltons ) t 0.00 Stsrt Tims ( M i m ) : t 0.00 End Tims ( Hins ) : Rspsats i 13.50 1 Channal Parent Daughtar Dwsll (Sees) Coli Energy (sV) Cone ( V ) 1 460.00 189.00 0.25 2 469.00 219.00 0.25 3 469.00 119.00 0.25 45 * 45 45 30 30 30 ] Punetlon l S MRM o f 3 Maas P a irs < ESP- ) In te r Channel D alay { Saca ) t 0.03 opan { D sltons ) i 0.00 S t a r t Tims < Hins ) t 0 .0 0 nd Tims ( H ins ) : 13.50 R spsats : Channel Parent D au g h tar 1 D w sll IS .e s ) C o l l E nergy (aV) Cons ( v ) 1 569.00 169.00 0.25 2 569.00 219.00 0.25 3 569.00 119.00 0.25 45 45 45 35 35 35 J P u n e tlo n i T MRM o f 1 K u a P a i r ( ESP- ) In ta r Channal Balay ( Saca ) : Span { S altona ) i S t a r t T in e | Mina ) < End T ina ( Mina ) i Rapaata > Channal P aran t Daughtar 0 .0 3 0.00 0 .0 0 13.50 1 Dwall . (Saea) C oll Enargy laV) Cons { v ) 1 427.00 0 .0 0 0 .2 5 40 40 } Pags l 000572 M asslynx Sample List Sample List: C:\M ASSLYNX\rats.PRO\Sam pleDB\030199c.SPL Printed: Mon Mar 0117:17:14 1999 Pagel File Name File T ext 1 030199001 MeOH Blank 2 030199002 MeOH Blank 3 030199003 Tox 120, RBL02229-H2O B lk -1 ,2/22/99 4 030199004 Tox 120, RBL02229-RBLIverBlk-1,2 /2 2 /9 9 5 030199005 Tox 120, RBL02229-5ppb-1,2 /2 2 /9 9 6 030199006 Tox 120, R B L 02229-10p p H , 2/22/99 7 030199007 Tox 120, RBL02229-25ppb-1,2 /2 2 /9 9 8 030199008 Tox 120, RBL02229-50ppb-1,2/22/99 9 030199009 Tox 120, RBL02229-100ppb-1,2 /2 2 /9 9 ' 10 030199010 Tox 120, R BL02229-250ppb-1,2/22/99 11 030199011 Tox 120, RBL02229-500ppb-1,2 /2 2 /9 9 12 030199012 Tox 120, RBL02229-750ppb-1,2/22/99 13 030199013 Tox 120, RBL02229-1000ppb-1,2 /2 2 /9 9 14 030199014 MeOH Blank 15 030199015" Tox 120 DNO. 1 2 5 F -G 2 ,2/22/99 D 5 16 030199016 Tox 120 DNO. 126F-G 2, 2/22/99 D 5 17 030199017 Tox 120 DNO. 127F-G2, 2/22/99 D5 18 030199018 Tox 120 DNO. 1 2 9F -G 3,2/22/99 D2 19 030199019 Tox 120 DNO. 130 F -G 3 ,2/22/99 D2 20 030199020 Tox 120, RBL02229-250ppb-CC1,2 /2 2 /9 9 21 030199021 MeOH Blank 22 030199022 Tox 120 DNO. 131F-G3, 2/22/99 D2 23 030199023 Tox 120 DNO. 132F-G3, 2/22/99 DZ 24 030199024 Tox 120 DNO. 133F-G 3, 2/22/99 D2 25 030199025 Tox 120 DNO. 1 3 4F -G 3,2/22/99 D2 26 030199026 Tox 120 DNO. 135F-G3, 2/22/99 D2 27 030199027 Tox 120, R BL02229-250ppb-CC2,2/22/99 28 030199028 MeOH Blank 29 030199029 Tox 120 DNO. 1 3 6F -G 3,2/22/99 D2 30 030199030 Tox 120 DNO. 13 7 F -G 3 ,2/22/99 D2 31 030199031 Tox 120 DNO. 138F-G3, 2/22/99 D2 32 030199032 Tox 120 DNO. 1 3 9F -G 3,2/22/99 D2 33 030199033 Tox 120 DNO. 141F -G 3 ,2/22/99 D2 34 030199034 Tox 120, R BL02229-250ppb-CC3,2/22/99 35 030199035 MeOH Blank 36 030199036 Tox 120 DNO. 142F -G 3,2/22/99 D2 37 030199037 Tox.120 DNO. 143F -G 3,2/22/99 D2 38 030199038 Tox 120, RBL02229-250ppb-CC4,2/22/99 39 030199039- MeOH Blank 40 030199040 Tox 1 2 0 ,106F-G1-250ppb-MS, 2/22/99 41 030199041 Tox 1 2 0 ,106F-G1-250ppb-MSD, 2/22/99 42 030199042 Tox 120, RBL02229-250ppb-CC5,2/22/99 43 030199043 MeOH Blank 44 030199044 Tox 120, RBL02229-H2O B lk -2 ,2/22/99 45 030199045 .Tox 120, RBL02229-RBUverBlk-1,2 /2 2 /9 9 46 030199046 Tox 120, R BL02229-5ppb-2,2/22/99 47 030199047 Tox 120, RBL02229-1 Oppb-2,2/22/99 48 030199048 Tox 120, RBL02229-25ppb-2,2/22/99 49 030199049 Tox 120, R BL02229-50ppb-2,2/22/99 50 030199050 Tox 120, RBL02229>100ppb-2,2/22/99 51 030199051 Tox 120, RBL02229-250ppb-2,2/22/99 52 030199052 Tox 120, R BL02229-500ppb-2,2/22/99 53 030199053 Tox 120, R BL02229-750ppb-2,2/22/99 54 030199054 Tox 120, RBL02229-1000ppb-2,2/22/99 MS File In let File TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A . TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A ' TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TO X120A .-x TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A TOX120A long2 long2 long2 long2 long2 long2 long2 long2 long2 k>ng2 long2 k>ng2 long2 . long2 long2 long2 long2 long2 long2 long2 k>ng2. long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 . long2 long2 tong2 k>ng2 long2 long2 long2 long2 long2 long2 B ottle 91 91 1 2 3 4 5 6. 7 8 9 10 11 91 12 13 14 15 16 17 92 18 19 20 21 22 23 92 24 25 26 27 28 29 93. 30: 31 32 93 33 34 35 93 36 37 38 39 40 41 . 42 43 44 45 46 Factor 1 Sampl 0 Analyti 0 Analyti 0 Analyti 0 Analyti 0 Stande 0 Stande 0 Stande 0 Stande 0 Stande 0 Stande 0 Stande 0 Stande 0 Stande 0 Analyti 0 Analyti 0 Analyti 0 Analyt 0 Analyt 0 Analyt 0 Analyt 0 Analyt 0 Analyt 0 Analyt 0 Analyt 0 Analyt 0 Analyt 0 Analyt 0 Analyt 0 Analyt 0 Analyt 0 Analyt 0 Analyl 0 Analyt 0 QC 0 Analyl 0 Analyt 0 Analyl 0 QC 0 Analyt 0 Analyt 0 Analyl 0 QC 0 Analyl 0 Analyl 0 Analy 0 Stand 0 Stand 0 Stand 0 Stand 0 Stand 0 Stand 0 Stand 0 Stand 0 Stand " [ Z u r . V \ |V \a J > 4 i V^U. 000573 FACT: DATA REVIEW SUMMARY FORM BESTCOPYAVAILABLE Date: Analyst: ci-rt FACT StudyNumber ' T h 't I^ J Q Analyte 4: ~$2A A Acceptable Linear Range: --' Jj Matrix Time Points toys l3 LOQ for this data set / D Re-evaluated for different range? f \ ) ^ Dilutions? S ia - Analyte 1: Pfc^L Acceptable Tihren*Range: Analyte 5: T - e J V T ^ M la i Acceptable LinearRange^ / c o - J t C C D p f b LOQ for this data set LOQ fix Ibis data set: j b Re-evaluatedfor differentrange? f\)o` Re-evaluatedfor different range? $ D Analyte 2: WEE Acceptable Linear Range], / O ' l < ^ o p p b LOQ for dns data set: /O ffe Re-evaluated fix different range? (Jo An junGaklxyjtve* v6.: tpfah* ^'gJyw tv --SjCa*i/ Acceptable E faggf^ ^e: LOQ for this data set Re-evaluated fix different range? a /a*d _ feloh cLclVc 0* Analyte3: Acceptable Linear Range: " / OC& o p b LOQ fix this data set Re-evaluated fix different range? lO^ Analyte 7: Acceptable LinearRange: LOQ fix this data set ~~ Re-evaluated for differentrange? 000574 vs~^ o t RS 7 " S SSSSSSSaSSSSSSSSSSSSSSSSSSSa Fi2gS3SS3S3SSpg2Sg3^2S?2222S2ESSSi:SS33SSS?gSS2SSSSaS2SS s - o` d s i i s s g s g E S " ^ " o,3 d s o' s s s 3 d H " a ' " s a E " d S " s s 8 " , ; -;,,!a a 3 2 8 g g V 2 IHHrIHHi i|5 liM s ll||ip S S lla p lS S a il5 l 8 lp il|3 |ip llls ls i!||i, > S :S H S p .p 3 S iS 3 p ie g :3 p S 3 s :S H iS S H S p ^ iiiiS S S S H p . sssssssss s s s g g sssssssss ' s S S jj i i S S "SSSSSSS5 l | | | | l | ! ! p aaaaal aaaaag aaaaal ,, g | p P . | | | | | | | l | Uh 4** i s f iS 32 h |s |3 Isis iW ? I ! ~i i ! 3 s S f f l W i ! 1 1 1 '* S ` - il! 'W W W I S jj a a a a a a lla 3 | s a ||s ! s a ,| |8 |a j is .s ia i 8 a a S i S 5 ` S5's` 5 ' S ' 5 S ' a 5 5 ' a 5 5 a a 8 3 S 5 5 a 5 5 ' ; S 5 ' 5 ; S S S S 5 5 a 5 5 5 5 lIlSHlSlSSilllSHlSSllMlllSSll1 I V g I W1 lli liii) lil 'S a a 3 3 3 S 5 S 3 S S a S S S S 5 S 5 S 2 S !3 2 S g P ;S 5 S i3 5 5 S S E S 3 S S S 2 S W rs. in o o o 1041098:: q u an titafcad and p rin ta d 0 3/08/99 by drb 9 r l t t N O l O H V r l 4H II I i (4 1 a a 3S2232SSSS s " -- 33333 4 H H H rrH H H H H i H H S jg H rl a .s r*- 3 NN1 a*> 2 * i w4 H H ! 3 u 3 S 3 SSSSoooIS "SSS2SSSS s s t jf|piiiill11i|ff|| ****** I 3 s" a aa ?aa ro- <on 3 3 ? e o oMtf)oo<H O O f4<hO M 4 e lMA H a la -3 3 3 5 3 3 2 3 iii " S*5H|S, 5 K3S SS SS s S S S s s S s K a 3o33ooSoo ' 'S S H jj 1 l ? p l | | | p sasaa s a s s s a a aSS ..i i! i i i i l i l i 3333' 3333 ffiiili lilil lilil lili if' 1 * 51 I I 8 1 I I 41MM " SS * - 3 a a 3 3 3 3 3 S 3 3 * ag3a3s3s2a as;si a; 3a3s3s3s Ss 3s ^s ^s s s s s s s s s s a s s s a < r ir> o o o 141098:: q u a n tita ta d and p r in ta d 0 3 /08/99 b y d rb TOX 120 BHO B a t L iv a r Ocoups 2 C I >041098! : q u a n ti t a t a d a n d p r i n t a d 0 3 /0 8 /9 9 lay 4 < t J 7" ' 1 533333 I sisals 3 m ai J .2 i s^ 2 3 tnH in rH- 3 0 " ^ 7 3 3 s 333 ** 333333 arlt mr- - s S S 3 lrAjoivnwtlBffNiH' araitt rn4 < 3 333 NNojrfntllOOoOQvleH 4 H *-t 4HH rlHHHHH r-# 1 i s s s H SSI3I VMHOrtH(MiHwNrwt NAe im s s * i m rin no nu n . ... $. & llBllllllallllllsilllallla SS393S sssssgsss -sssssssis 3 3 s oH - isisasiiill....1 11aaaaal aaaaal aSaaal aal 111IpSpIllt 1 4 l l ....... a a a 5 S S S S 'S 5 S '= 3 3 5 S S S S S 3 S 5 a 3 3 S ';a 5 5 2 n S " 3 5 S 3 i i J < J 2 <<(<<3 l i 2 2 <<2 l < i J l l 3 l < i i < J i i l 2 2 J3 l I 2 1 2 l < l 2 2 l p* K oIn o o 141098: : q u a n tita te d and p r in te d 03/08/99 by deb O O o C/l OB 8S88888 Ko)oKo) NoMooK o) N*M-U* ................... 5ir 1888 888 8 8 8 8 8 SS8 8 8 8 8 8 I _ H* H* I--M H* MO O O O O O tH0QORO OtO4OMMV * s i g m *S S'b H I H * NoKt*s t)H*H<JMU*WUP*4*UHM4)(H*A4 ' K NME*0IUMj iUaWU*UM*Um* ?KBnSBBmB D* * * * Ko *BBB MoKoloKol MoNoMwViI ...................6 ! B S S S B B "'' SEBEES BBBoB ft* 7TJNJ KNJ KMJNt J JNJ *.8)i>00 0W 00 0 w SgBBBB q vk. S k ks.kv. H 0 0 00000 C>0B B 8 8 S NMNMSMNNMNS MNS SS i00iH00i00.0ti al ia H00 00t t0W00NMOH0 t0NMH I )O OO O O I MUa MeU0uU4AU*MUuUK0*)Uu1U0A 0 U 4a UNM rIO* / H HHM 3 4 K) /NUUIOHUAU. Mt A 0aaN *ea HO HHH Oh 4A*1 <400 OD U0U000 l00 e 00A0U0 OW0 0<4<40H HHHHHH 4HU4A 00M0*4<40 S&&SS5SS e M4M4M*J SMO 4Hhi S5& S 5 6 U0O000M0000OAM M0JlJ<<4J & H *m m H 00 0W0NNHW N H 0000O 00M I J: g i J14 UUKJM)l lW0U00U0WUWUUU0M w* mh w oo H,,M A0UH wSSSStSIii HUVbH 00HO0M M MUHHAHAM Ss? MMg 5 ffI Q uantify Coapound Suanaxy R aport teat 120 DHO R a t L iv ac G roups 2 6 3 S aap la L i s t : M:SBAIS.8R0\.1aspTarB\030i99o b a s t n o d i f i a d : Man M ar 08 0 9 :4 9 :2 1 1999 lia th e d : M :\ratx.SRD\HathDB\030199a b a s t n o d i f i a d : Mon M ar 08 1 0 :0 3 :3 2 1099 Job Coda: P rintad: Mon M ar 08 1 0 :3 3 :4 9 1999 Paga 3 Coapoiad S : TalaarlSO Wane f a lla l 1st ta rt 1 030199001 MaOH B lan k 2 030199002 MaOH B lan k 3 030199003 T o r 120, BBL02229-H20 B lk -1 , 2 /2 2 /9 9 1 030199001 Tox 120, BBb02229-BBbivarBlk-l, 2 /2 2 /9 9 S 03019900S Tox 120, BBM2229-Sppb-1, 2/22/99 6 030199006 Tox 120, B8I02229-10ppb-l, 2/22/99 7 030199007 Tox 120, BBL02229-25ppb-l, 2/22/99 0 030199008 Tox 120, 9BL02229-S0ppb-1, 2 /2 2 /9 9 9 030199009 Tox 120, HBL02229-100 p p b -l, 2 /2 2 /9 9 10 030199010 Tax 120, XB02229-250ppb-l, 2 /2 2 /9 9 11 030199011 Tox 120, BBl02229-500ppb-l, 2/22/99 12 030199012 Tox 120, BBL02229-750ppb-l, 2/22/99 13 030199013 Tox 120, m 0 2 2 2 9 -1 0 0 0 p p b -l, 2 /22/99 11 030199011 . HaOK B lank 15 030199015 Tox 120 DHO. 12SF-62, 2 /2 2 /9 9 DS 16 030199016 Tox 120 DHO. 126P-C2, 2 /2 2 /9 9 DS 17 030199017 Tox 120 DHO. 127F-G2, 2 /2 2 /9 9 D5 18 030199018 Tox 120 DHO. 129F-G3, 2 /2 2 /9 9 02 19 030199019 Tox 120 DHO. 130F-G3, 2 /2 2 /9 9 D2 20 030199020 Tox 120, BBL02229-2S0ppb-CCl, 2 /2 2 /9 9 21 030199021 MaOH B lank 22 030199022 Tox 120 DHO. 131H-G3, 2 /2 2 /9 9 D2 23 030199023 Tox 120 DHO. 1321-03, 2 /2 2 /9 9 D2 24 030199024 Tox 120 DHO. 13 3 r-C 3 , 2 /2 2 /9 9 D2 25 030199025 Tox 120 DHO. 13IF-G 3, 2 /2 2 /9 9 D2 26 030199026 Tox 120 DHO. 13SF-G3, 2 /2 2 /9 9 D2 27 030199027 Tox 120, RBb02229-250ppb-CC2, 2 /2 2 /9 9 28 030199028 MaOH B lank 29 030199029 Tox 120 DHO. 136F-63, 2 /2 2 /9 9 D2 30 030199030 Tox 120 DHO. 137 1 -0 3 , 2 /2 2 /9 9 D2 31 030199031 Tox 120 DHO. 138F-G3, 2 /2 2 /9 9 D2 32 030199032 Tox 120 SNO. 139F-G3, 2 /2 2 /9 9 02 33 030199033 Tox 120 DHO. 141F-03, 2 /2 2 /9 9 D2 34 030199034 Tox 120, RBb02229-2SOppb-CC3, 2 /2 2 /9 9 35 030199035 MaOH B lank 36 030199036 Tox 120 DHO. 112F-G3, 2 /2 2 /9 9 D2 37 030199037 ToX 120 DHO. 143F-G3, 2 /2 2 /9 9 D2 38 030199038 Tox 120, RBL02229-2S0ppb-CCI, 2 /2 2 /9 9 39 030199039 MaOH B lan k 40 030199040 Tox 120, 106F-01-250ppb-MS, 2/22 /9 9 41 030199041 Tox 120, 106F-G1-25Oppb-MSD, 2 /2 2 /9 9 42 030199042 Tox 120, BBb02229-2S0ppb-CCS, 2 /2 2 /9 9 43 030199043 - MaOH B lan k 44 030199044 Tox 120, BBL02229-H20 B lk -2 , 2 /2 2 /9 9 45 030199045 Tox 120, BBb02229-BBblvarBlk-l, 2/2 2 /9 9 46 030199046 Tox 120, RBb02229-5ppb-2, 2/22 /9 9 47 030199047 Tox 120, BBL02229-10ppb-2, 2/22 /9 9 48 030199048 Tox 120, HBL02229-25ppb-2, 2 /2 2 /9 9 49 030199049 Tox 120, BBL02229-50ppb-2, 2 /2 2 /9 9 SO 030199050 Tox 120, BBb02229-100ppb-2, 2 /2 2 /9 9 51 030199051 Tox 120, BBL02229-2S0ppb-2, 2/22 /9 9 52 030199052 Tox 120, BBb02229-500ppb-2, 2/22/99 S3 030199053 Tox 120, BBbO2229-7S0ppb-2, 2 /2 2 /9 9 54 030199051 Tox 120, BBW2229-1000ppb-2, 2 /22/9 9 * S td Cono A nalyt RS A nalyt A nalyt A nalyt S ta n d s 5.99 S ta n d s 12.00 S ta n d s 29.90 S ts n d s 59.90 S tan d s 120.00 8.571 S tan d s 299.00 S.S49 S tands 599.00 8.593 S tan d s 898.00 8.562 S tan d s 1198.00 . 8.541 A nalyt A nalyt 8.150 A nalyt 8.168 A nalyt 8.149 A nalyt 8.361 A nalyt 8.340 QC 2 9 9 .0 0 8.599 A nalyt A nalyt 8.370 A nalyt 8.553 A nalyt 8.371 A nalyt 8.540 A nalyt 8.552 QC 2 9 9.00 8.559 A nalyt A nalyt 8.352 A nalyt 8.331 A nalyt 8.572 A nalyt 8.568 A nalyt 8.585 QC 2 9 9 .0 0 8 .5 6 3 A nalyt A nalyt 8.572 A nalyt 8.559 QC 2 9 9.00 8.568 A nalyt A nalyt 8.580 A nalyt 8.560 QC 2 9 9 .0 0 8.5 0 5 A nalyt A nalyt A nalyt S te n d a 5.99 S tatida 12.00 Stenda 29.90 S te n d a 59.90 Stenda 220.00 8.536 Stenda 299.00 8.550 S tenda 599.00 8.546 S tenda 698.00 8.505 Stenda- 1198.00 8.578 A rs a D U .F a c t. Cono F la g * %Dev 86 1 27S 1 372 1 631 1 727 1 311 1 301 1 266 1 329 1 418 1 173 1 281 1 4(5 1 260 1 352 1 500 1 163 1 391 1 380 1 408 1 357 1 328 1 262 1 257 1 218 1 222 1 226 1 196 1 190 1 119 1 209 1 393 1 535 1 703 1 X 8 5 .1 4 MM 4 1 9 .5 1 bbX 5 9 2 .4 3 MM 1 0 4 9 .4 9 MMX 1220.49 bb 4 8 3 .6 5 MK 4 6 5 .1 7 MK 403.94 bb 5 1 4 .8 4 'bb 7 2 5 .7 9 MK 23B .58 MK 430.52 bb 7 2 0 .9 0 MM 393.56 bb 5 5 6 .1 9 MM 8 ia .12 bb 2 2 0.94 MK 6 2 5 .6 7 MK 605.50 bb 6 5 4 .8 5 MK 564.48 bb 513.91 bb 3 9 7 .3 4 MM 3 8 8 .5 0 MM 319.39 bb 3 2 5 .7 9 MK 3 3 3 .8 2 MK 2 7 9 .8 7 MK 2 6 8 .6 1 MM . -29 40 -1 17 2 \ \ \ \I -20 / /I /1*b.-hwL-t. t_AJ. r/ 0 3 / oj -26 - \ \ \ I A 33 | j / / 9_ // -10 144.01 bb 302.82 bb 6 2 8 .6 2 MK 879.50 bb 1177.99 bb 20 1 5 -2 -2 % 3A t r ilt r ii, 7^1 (lloooil^ COsrk chicli. LS Wil'L'U. Cfiltrf.+ hrailhj. ewwlo. Qflkft. is Ok fl/lA Urtjorialjli., W e - o j / o j lq<\ ? /fi/Ojpfcc. Hd^Usi adelinaO ilQ O O : t q u a n tita te d a n d p r in te d 0 3 /0 8 /9 9 b y d rb 000579 4t a e cm t a m 1 1 CM 0 CM 0 1 1111 ? sU CM CM t a CM m 0 c e 0cm a s1 0 H M A m i t a o h cm a 0 t a <-4 CM CM 0CO II t3a i HHHHHH t a <0 49 40 49 m H CM CM A t a O H CM CC 49 0 i f l 0 A 0 O 0 *4 S H N H N O AAAAA AO O O O O O O O g A O A A eeeoo 3 0CM A A O A AA A 4CM 0C M A A AA * 4 CM 0 A >4 3 C0 0t 33 taA 40 m CM CM 4P m H CM CM g CM 0 A CM CM ta 0 CM H 11 0 SS3 a wm 0 IM O CM A A CM CM H CM S3 H CM tn 0 00 Ns 5S3 0 CM H aa e CM CM O 0w m NHH A A K) h, CM CM 40 777 S 3 3 3 0 O CM t a CM 0 A t n 0 40 (M 40 0 0 0 0 CM CM A CM 0 CM 40 4 O . A * 4 * H 0 0 0 ta HH 0 40 40 0 CM H H ta e M A A 0 *4 AA O e A A CM CM CM A e 0 A A CM H HH 40 A H M 0 0 *H H 00 00 O HH H 0 ta ta 0 m cm 0 0 cm H HH HH HH 0 CM CM 0 0 0 A 0 CM 0 t a A 0 CM 4 CM 40 * 4 t a 49 0 ta CM 0 CM AAA e e A A CM OA CM CM AA 0 ta 0 0N 0 AAA Oe eA AA AA CM CM ta H 0 0 0 0 e 00 0 <4 CM <4 0 0 000000 AAAAAAA OOOOOOOOO AO AAO O O O O 0CM A A O A A00 4CM 0CM A A AA H N 00H A A A t oAt AA A A NNNSSNA nN A Nn A Ms S nN r-Sni NM S ! M CM a a a *N N CM 0 OO0 O rAIi ANfAAIAHINAIiAnI CCMM CCMMCMM CCMM M CM CM CM CM . aasaaa iS iaaaa h N N ta ta A ssassam w R a o m N CM S" 3 8 H N NIMNCMN(MNNNCM NNNN^ CM CM CM CM CM m mptHaiNntaPntIaMntaCntMaCNA tatatatataA PlPIPlU^fj H H H r l H *' Il______ O O CI MMIm n cm iiiila*ggggga 3*gggggg iwOOOOOo o e o o o O O H O O O O O O r CM CM CM CM CM CM C M C M M C M C M C M C M C M C M I HrlHHHH a HHHH sasass s a s - s a s ;H H Hn H H HH t CM CM CM CM t3a H3 3H843N3Ht3a 8 ta 1 X t 3 at 8 at 8 at 3 at 8 at 81 aS t3at8a8ta8ta8ta8ta j5H3 K3 H3 HS H3 HS S MS 3> K8 f K3K3h8:; t CM A CM AA AA A I NS Ao A WA AS AN AS SA N*Sk I A SSN N N N N N N N M C iC C P IC C fC 's IH N N N N N N S S N I CM S N S CM CM CM + M CM M CM li- ft a ** > M CM CM CM CM I H CM CM CM ` tatatatatas*ai isisisisis**t r - m mA A A A A A CM CM CM CM CM CM CM CM CM CM 4 CM 3333333333 --gasaaaaa _OOOOOOOOO CMCMCMCMCMCMCMCMCMCM HHHHHHHHHH 88 8 3 8 3 3 8 3 3 3 HNH OV I O, O H N P I M AAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAoOA oOA oOA oOA oOA oOA eOAoOAwOA -OA. OAo OA' A A A A A A A A A A A A A A A A AOx .O........O........O........O........O........O........O........O........O.......-O ....O........O........O........O........O........C.......-. A_ A--A_ A--A-- A--A--A_ A--A--oA--o Ao- Ao Ao Ao oA oA cA A A A A A A A H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H H oooooooooooooooooooooooooooooo ooooooooooooooooooooooo i J rp--i i --O --f i -P ^> foi Po i on no poi oo Po Ho i Po oP oi Po i o Po Ho i ro t oP o r ot Po i o ioP oi 5of o 3o0 o2 2o 2o2 o ? o2 2o 2o 2o o2 o 2 o2 2o 2o So 2o o2 io2 o2 o2 o2 0o o2 2o 2o2 |N P |M C IM h A O H N P I ill< B h B A e H N P IM O I0 M }a e H N P IM iO V h a O lO H N n M ) r 4 H H H H H H H N N C I N M N P I W P | P | P | P J P l P | P | P H l1 P I M M M M M M M M M M i l H O l l l i n O 00 in o o o W *4 66/80/0 Wtrptd f a pawnTM** ::S60TI 141098:: q u a n tita ta d and p r ia ta d 01/08/99 b y dxb saBSSSSaSSSCSSSSSiSSSSSSSJSSKlgKSSSSKCKPS.-^.-. r I m m m m m iw iiw m m w iw w im m m m u gsggSSgSSgggggssssgsssSssgsgSsgBSsgsSsggsssgssgggsggssg i* ; ; r BBv * &V a V a &a &&* f !I1IB ilii IBJ % o * o % o * * s IIPX r r r r f**i*'l !lllllll5l sil Ssssss p p = bb S s b ' b S b b b b b B- bbbbb - 1111 til? SSS- S5SSS K! s i sssssssss n* OUe N(tNUOMOtM*fJ IfEKH &&**** VHHHMMHHM Oo Oo Oo Oo Oo Oo Oo Oo oO NV UO N tNf WH OUOU>NJNOU UU O o o en HH NH WH NH NO Hb^NO H 0O 0 MHHMKHMHH H N H M N H H M O U I* 9 H 9 O Hs 0 *# HM (?V 0 0 e o e OHOHHOOMOOO SSSP3S3K32 #- aas 0o 0UkOM-oNObU>WNOt9fa9H0 S333535S33* 3 3 3 33333333333 wi M iU,l w u .~ 1 Q uantify C a lib ra tio n R aport rox 130 BHO R a t L iv a r Seoupa 3 8 3 1 A llib ra ti on: M:\xata.SRO\CurvaDB\010199a ' M t n o d i i i a d : Mon Mar 08 1 0 :1 0 :0 7 199* Printed: Mon Mar 09 1 0 :3 S :0 S 1*99 I ] ] ] T ] i i J 3 ] 1 ! J I idalinaO U .098 : : q u a n tita te d an d p r in t a d 0 3 /0 8 /9 9 b y d rb i Raga 1 000582 Q u an tify C a lib ra tio n K ap ert TOC 1 2 0 aio K a t l i v m r C ro u p s 2 C 1 C a lib r a tio n : M :\sats.9B0\CurvaEB\O3O199e l a s t m o d ified : lion Iter 00 11:0<:32 190 P rinted: Mon Mas 08 1 1 :1 0 :0 7 1998 Paga 2 aa d elin aO 41098 : : q u a n tita te d and p r in te d 0 3 /0 8 /9 9 b y dab 000583 1 ifcify C a lib ra tio n E ap o rt 120 DHO S a t U v a s O roupa 2 0 3 1 a l it e r a t i o n : M: \ r a t a .JUACurva0B\030199o a a t a o d if la d : Mon H as 08 1 0 :1 0 :0 7 1980 T intad: I t e Mas 08 1 0 :3 8 :0 9 1399 1 I ] 1 T 1 .1 i I ] J ] ] .1 J ] m ad alin a0 4 1 0 9 8 : : q u a n tit a ta d an d p r in ta d 0 3 /0 8 /9 9 b y deb i Vaga 1 000584 Q u a n tify C a lib ra tio n Rapor t TOX 1 2 0 DHO R a t U v a s S c a u p s 2 C 3 C a lib ra tio n : M :\cats.9RO\CumOB\03Q199a L a s t a o d ifia d : Mm M u 08 10:10:07 1908 P rintad: Mon MU 08 1 0 :3 0 :0 3 1899 Compound 4 name: POAA Correlation coefficient r = 0.998817, r*2 = 0.997636 Calibration curve: 5.20938 * x +18.1144 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: Null, Axis trans: None Pag* 4 m * d u lin a 0 4 1 0 9 8 :$ q u a n t i t t a d a n d p r i n t e d 0 3 /0 8 /9 9 b y dadi 000585 Quantify Calibration Hapcct TOX 120 OHO Hat Livar Sroup 2 c 3 Calibration: M: \rata.9H0\CuxvuCB\010199a last aodiflad: Mon Mar 03 10:10:07 1399 Prlntad: Moo Mar 08 10:38:03 1999 paga 5 aadalina041098:: quantitatad and psiatad 03/08/99 by drb 000586 1 lu an tify C a lib ra tio n R apact fCflC 1 2 0 OSO R a t U v n C r o u p * 2 ( 3 1 la lib r a tio n ; M :\rats.IR O \C u rv tfB \0 3 0 1 9 9 a * * t a o d i f i a d : Mon Max 00 1 0 :1 0 :0 7 1900 fein tad : Mon Max 09 1 0 :3 0 :0 3 1990 1 C om pound 6 nam e: Telm er569 C orrelation co efficien t r = 0.997982, r* 2 = 0.995968 C alibration curve: 2.28567 * x + -17.6540 1 R esponse type: E xternal Std, A rea C urve type: Linear, O rigin: E xclude, W eighting: N u ll, A xis trans: N one ] j 1 1 i I ] J 3 ] ] I ] 1 td elin * 0 4 1 0 9 8 :: i{ u a n tiU ta d and p r tn ta d 03/0 8 /9 9 b y drb ii Saga ( 000587 Q u an tify C a lib ra tio n B a p e rt TOX 1 2 0 OHO B a t U n r C r o u p s 2 0 3 C a lib r a tio n ! M :\rats.B 8 0 \C u rv aB B \O lO 1 9 9 o L a a t a o d if ia d : Mon M ar 01 1 0 :1 0 :0 7 1390 B rin ta d : Mon M ar 00 1 0 :3 0 :0 9 1999 7 aadalina041098:: q u a n tita ta d and p rin ta d 01/08/99 by dsb 000588 M ethod R e p o rt M ethod f i l e ! L a st m o d ified : Compound: P rin te d : M :\rats.P R O V M athD B \030199e.m db Hon M ar 09 1 0 :0 3 :5 2 19990 1 : P90S KOn M ar 09 1 0 :1 0 :0 2 1999 Compound Hio u i In tarn al R af.: Q uantify Traca: Cone, o f S tandards: U sa r RF V a lu o : Usar Paak F actor: I n t a g r a t a Window F a c to r : Paale L o c a tio n R atantian Tina (B ins): RaXativa R atan tio n T ina: T in s Window (m in s): Paale S s ls c tl o n : Raaponaa Rasponsa Typa: Raaponaa: C a lib ra tio n Curvaa Polynom ial Typa: P o in t o f O rigin: F i t W aighting: A xis Tranaform ation: C oncantratlon Units: Kola a Paak-to-paak am plituda: SBOOth Sm oothing: Window a i z a ( s c a n s ) : a Huabsr o f aaooths: Smoothing mathod: B aaallnas Jo in v a lla y thrashold: Raduca paak ta ilin g : R a is a b a s a l i n a maximum: v Paak S aoaration Draw v a r t i c a l th r a s h o ld : D atact shouldars: Shouldar th ra sh o ld : Rasponsa Thraahold R alativ a H aight: A bsoluts H aight: R alativa araa: A bsoluts araa: nos (Mona) TIC Cone. A 1.000000, D isablad 1.000000 2.000 0.130, Inablad 0.000, D isablad 0.793 F aarast S x ta rn a l A raas L in aa r Ix c lu d a Rons Mona 150 D isablad 3 2 2 0 .0 0 100.00 0.00 10.00 D isablad 10.00 1.50, D isablad 0.00, D isablad 2.00,* D isab la d 00.00, Inablad Peg* 1 OHI0W Uc o i l o s h i A 000589 M ethod R e p o rt M ethod f i l e : t e a t m o d ified : Compound: P rin te d : H :\nto.IIl0\ltethia\0301M e.adb Hon H er OS 1 0 :0 3 :5 2 19990 2: m s Hon H er 09 1 0 :1 0 :0 2 1999 Compound Mama: In tern al R ef.: Q uantify Traee: Cone, o f Standards: PfHS (Nona] TIC Cone. A U sa r RF V a lu a : Usar Paak fa c to r: I n t e g r a t e Window f a c t o r : Paak Location R eten tio n Time (m ine): R e la tiv e R eten tio n Time: Time Window (m in s): Paak S election: Response Response Type: Responses 1.000000, Dlsabl .1.000000 2.000 5.732, In ib lad 0.000, D ijablad 1.109 V aarast ' Ixtam al A reas C a lib ra tio n Curves Polynom ial Types Point o f O rigin: f i t W eighting: A xis Transform ation: L in ea r Include None Stone C oncentration U nits: N o ise Peak-to-peak am plitude: 290 Smooth Smoothing: Window s i z e ( s c a n s ) : . Number o f sm ooths: Smoothing method: D isabled 3 2 B aselines Jo in v a lle y threshold: Reduce peak ta ilin g : R a ise b a s e l i n e maximum: 0.00 100.00 0.00 Peak Seoaration Draw v e r t i c a l th r e s h o ld : 10.00 D etect shoulders: D isabled Shoulder th re sh o ld : 40.00 Response Threshold R elative h eight: A bsolute h e ig h t: R elative are: A bsolute a rea: 1.50, D isabled 0.00, D isabled 2 .0 0 / D isabled 10.00, Enabled Page 2 Mank lw.. cwoy______ i m .oiIm Ivi 000530 M ethod R e p o rt M ethod f i l e : L a st m o d ified : Compound: P rin te d : M:\ r a t s . PR O \H ethD B \0 3 0 1 9 9 e.m d b Kon M ar 00 1 0 :0 3 :5 2 1999Q 3: Kon Mar 08 1 0 :1 0 :0 2 1999 Compound Hi m : In ta m a l Ref. i Q uantify' Trace: Cone, o f Standards: [Mona] TIC Cone. A V sar HI V alua: Vsar Paak F actor: I n t a g r a t a Window T u t o r t 1.000000, D isab) 1.000000 2.000 Paak Location R atantion Tiaa tain s): R alativ a R atantion Tina) T in a Window (n in a )i 1.103, Xnablad 0.000, D isablad 1.000 Tank S o lu tio n : B aaraat Response Response Typai Response: K xtarnal A raas C a lib ra tio n Curvaa Polynom ial Typa: P o in t o f O rigin: f i t W eighting: A xis Transform ation: L in ea r Ixclw le Bone Bene C oncentration U nits: M oiaa Peak-to-peak am plitude: 1 Smooth S m oothing: Window s i z e (s c a n s ): Humber o f sm ooths: Smoothing method: D isabled 3 2 B aselines J o in v a lla y thraaK old: Raduca paak ta ilin g : R aisa b a sa lin a ariwna: 1 Task S atu ratio n 20.00 100.00 0.00 Draw v e r t i c a l th re s h o ld : D ataet shoulders: Shoulder th resh o ld : 10.00 D isabled 0.00 Response Threshold R alativa haight: A baoluta h aig h t: R alativa azaai A baoluta araa: 1.50, D isablad 0.00, D isablad 2 .0 0 ,'D isablad 00.00, Xnablad Rag 3 M a c U .W , DM1DM A t. m / m / w 000591 M ethod R e p o rt M athod f l l : L a s t m o d ified : Com pound: P rin te d : H :\rats.P R 0 \H eth D B \0 3 0 1 9 9 c.m d b Hon Ite r 06 1 0 :0 3 :5 2 19990 I : POM Mon M ar 08 1 0 :4 0 :0 2 1999 Compound N ana: In tarn al R ef.: Q uantify Trace: Cone, o f S tandards: PQAA [None] . TIC Cone. A U s e r RP V a lu e : U ser Paak fa c to r: I n t g r a t Window F a c to r : 1.000000, D isabled 1.000000 2.000 Paak Location R etention Tina (n in e): R elativ e R etention Tina: T in e Window ( n in e ) : 6.624, Snabled 0.000, D isabled 1.000 Paak Selection: D earest Response Response Type: Response: In te rn a l A reas C a lib ra tio n Curve Polynom ial Type: P o in t o f O rigin: l i t W eighting: A xis Transform ation: L in ea r Kxclude Done Hone C oncentration Units: P o is e Peak-to-peak am plitude: 107 Smooth Sm o o th in g : Window s i z e ( s c a n s ) : . Humber o f sm ooths: Smoothing method: D isabled 3 2 B aselines Jo in v a lle y th resh o ld : Reduce peak ta ilin g :. R a is e b a s e l i n e maximum:.* 2 0 .0 0 100.00 0.00 Peak Separation Draw v e r t i c a l th re s h o ld : D etect shoulders: Shoulder th re sh o ld : 10.00 D isabled . 40.00 Response' Threshold R elative h eig h t: A bsolute h e ig h t: R elative area: A bsolute are a: 1 .5 0 , D isabled 0.00, D isabled 2 .0 0 , `D isabled 60.00, D isabled Pag 4 MadfeL, omoqj___ ik e . m I m / m :X 000592 M ethod R e p o rt M ethod f i l e : L a st m o d ified : Coapound: P rin te d : M :\rats.PRO\M ethDa\030199c.m db Ksn Mer 08 10:03:32 19990 3 : T elm art< 9 Mon M ar 08 1 0 :1 0 :0 2 1999 Coapound Hama: I n ta rn a l Hof: Q uantify Traca: Cone* o f S ta n d a rd s : U s e r MT V a lu e : User Peak F actor: I n t e g r a t e Window f a c t o r : Peak lo c a tio n R etention Tine (B ins): R elativ e R etention Tine: Tima window ( n in s ) : Paak Salaction: SUsDcnsa Rasponsa Typa: R tapons: C a lib ra tio n Curvas Polynom ial Typa: Point o f O rigin: f i t W eighting: A xis T ransform ation: C oneantration u n its: K o isa Peak-to-peak am plitude: Smooth S m oothing: Window s l z a ( s c a n s ) : . Nunbar o f sm ooths: Smoothing nath o d : B asallnas Join v allo y threshold: Radueo peak t a i l i n g : R a isa b a s e l i n e maximum:.' Paak S a tu ra tio n Draw v a r t i e a l th ra s h o ld x D atact sh o u ld ars: Shouldak th ra s h o ld : kasDonsa T hrashold R alativa h aig h t: A bsoluta h a ig h t: k alativa araa: A bsoluta a ra a: Talaar469 IHona) TXC Cone. A 1.000000, D isabl 1.000000 2.000 0.370, Rnablad 0.000, D isabled 1.000 V aarast a In tern al A reas L ln aa r Ix c lu d a Kona Hona 169 D isablad 3 2 20.00 100.00 0.00 10.00 1 D isabled . 0.00 1 .50, D isabled 0.00, D isabled 2.00,' D isabled 00.00, Rnablad Macl&Li QKtoM \ A c b ih x lw Page 3 000593 M ethod R e p o rt M ethod f i l e : L est m o d ified : C om pound: P rin te d : M: \ra ts.P R O \M sth D 8 \0 3 0 1 9 9 c.a d b Mon Mar 08 1 0 :0 3 :5 2 1099a 6: T e la e rS < 9 Mon M ar 08 1 0 :1 0 :0 2 1999 Compound Ham! In tern al R tf. s Q uantify Traea: Cone o f S ta n d a rd s ) T alm ar569 [Hone] TIC Cone. A U se r R7 V a lu e : User Peek F actor: I n t e g r a t e Window f a c t o r : 1.000000, D isab led 1.000000 2.000 Saak Location R etention Tine (nlns): R elative R etention tin e : T in e Window (m in s): 9.818, Bnabled 0.000, D isabled 0.500 Peak S electio n : V earest Resocnse Response Type: Response) E x tern al A reas C a lib ra tio n Curves Polynom ial Type: Point o f O rigin: P it W eighting: A xis Transform ation: L in ea r Exclude Home Rene C oncentration U nitst B o ise Peak-to-peek an p litu d a: . 169 Smooth Smoothing: Window s i c e ( s c a n s ) : Kuaber o f smooths: Smoothing method: D isabled 3 2 B aselines Jo in v a lle y threshold: Reduce peak t a i l i n g : R a is e b a s e l i n e maximum: . 20.00 100.00 0.00 Peek Separation Draw v e r t i c a l th re s h o ld : D etect shoulders: Shoulder th re sh o ld : 10.00 4 D isabled 40.00 Response Threshold R elative h eig h t: A bsolute h e ig h t: R elative area: A bsolute a re a: 1.50, D isabled 0.00, D isabled 2 .0 0 ,.D isabled 00.00, Inabled MorlA). CH UM ___ LAC- Q l l p t f a leg e 6 000594 M ethod f i l e : L e st m o d ified : Compound: P rin te d : H :\rata.P R O \H eth IIB \0 3 0 1 9 9 c.m d b Mon M u 01 1 0 :0 3 :5 2 19990 7: su rr Mon M er 01 1 0 :1 0 :0 2 199 Compound V iH t I n tu n e l K ef.: Q uantify Trace: Cone, o f S tandards: U se r RP V a lu e: User Peak Factor: I n t e g r a t a Window T a c to r : Peak lo c a tio n R e te n tio n Tima (m ins): R e la tiv e R eten tio n Time: Time Window (m in s): Peak S election: Response Response Type: Response: C alib ratio n curves Pclynom ial Type: Point o f O rigin: T it W eighting: Axis T ransform ation: C oncentration U nits: B o ise Peak-to-pak am plitude: Smooth soothing: Window s i z e ( s c a n s ) : Humber o f sm o o th s: so o th in g method: B aselines Jo in v a lle y threshold: Reduce peak ta ilin g : R aise b a s e lin e maximum: Peak Seoaration Draw v e r t i c a l th r e s h o ld : D ateet shoulders: Shoulder th resh o ld : Response Threshold R slative height: A bsoluts h e ig h t: R elative aree: A bsoluts a rsa: s u rr [Bone) TIC U sed 1.000000, D isabled 1.000000 2.000 7 .3 0 0 , Xnabled 0.000, D isabled 1.000 H auest ' Internal A reas lin ear Include Bo m Hens 169 D isabled 3 2 20.00 100.00 0.00 10.00 D isabled 10.00 1.S0, D isabled 0.00, D isabled 2*00,. D isabled 00.00, b a b ie d M a A t L - Mici? u c oiloaln 000595 AM ELIA062498: FACT Equipm ent L og 98061 Q uattro n , #6448E PAGE DATE: 03/16/99 ANALYST: hoi ' STUDY NUM BER to xl20. MATRIX: R at liver D ESCRIPTION; ion pair dilutions FACT M ethod: FACT-M -4.0 Injection volum e.10 uL Cycle time: 13.5 m in. Electrode: Z-Spray M obfle P hase: (A12.0mM NH4CH3CQ2 (BIM eO H TN -A - or stndrd num ber (A ) 98094-15-20________ . (B1TN-A-2325 Prepared (date/by): E x p ires: ( A) 3/16/99 hoi__________ ( A) 09/99_______________ 0313/16/99 hoi (S ) 9/16/99 Store at room tem p? Q o r N O ther G u ard colum n: N one___________________ P art num ber: na_________ Lot number na A nalytical colum n: keystone b e ta sil___________;__ Size: 2 x 100mm________________ Type: c l 8___________ _ Sphere size: 5 um Part num ber 105-701-2_______ L otnum ber__JP8H 08 Serial num ber 02949SD A nalytical param eters: Drying gas (L /hrl: 300 ESI nebulizing gas (IVhr) 15 LC Flow rate: 300 uL/m in. B ackpressure: 100 b ar Sheath gas (L/hr)_0___ HPLC solvent gradient: long2 Tim e (m in.) 11 0.00________ 21 8.5 3 11.0_________ 51 12:5 6113.5_________ %B 40 90 90 40 40 000596 ^ Tuning Method Report : ________ Method: C :\MASSLYNX\RATS2.PRO\ACQUDB\PFOS Printed: Tue Mar 16 09:59:43 1999 _ ___________________________________ _____ _____________ .I A to L * n i M V i Page 1 iSTCWmtlMLE MS SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. Dau 499.00 Set Rdbk 3.00 60 5 0.2 150 .250 2.99 -60 -6 150 258 Pressures Analyser Vacuum Gas Cell Rdbk 1.0e-4 4.5e-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier .*S. 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 ' 56 650 Set Rdbk 15.0 15.0 45 2.0 0 .0 40 0 650 46 38 46 000597 S c a n n in g M ethod S o p o ri M ethod: C:\HMStTJOC\RAI32. s R o u c o u B a w r o a - p n s -M L a a t M o d ifie d : Mem M ar IS 1 3 :2 3 :3 3 1999 P rin te d : Too M ar 1 1 0 :3 3 :3 1 IM S Solvent D elay < a la s ) i 0 .0 0 function : 1 MRM o f 4 M aes f a i r s ( ZAP- ) I n te r Channel D elay ( Secs ) l Span ( D eltona I t S ta r t Tine ( K ins 1 t End T ine ( K ins ) i R ip ilti S Channel P aren t D aughter 0.03 0.00 0 .0 0 13.30 1 D w ell (S ees) C o ll E n e rg y (eV) Cone < V ) 1 499.00 0 .0 0 0.40 2 499.00 99.00 0 .4 0 3 499.00 130.00 0.40 4 499.00 180.00 0.40 45 4S 45 45 0 SO SO SO Function t 2 MRM o f 4 M ass f a i r s 1t S f - 1 In te r Chennai D elay I Secs ) i Span ( D altons ) : S ta r t T ina ( Kina 1 : End T ine ( H ina ) I R epasts : Channel P aren t Daughter 0 .0 3 0 .0 0 0 .0 0 13.30 1 D w ell (S ecai C o ll E n e rg y (eV) Cone ( V ) 1 3 9 .00 0 .0 0 0 .4 0 2 399.00 99.00 0.40 3 399.00 130.00 0.40 4 399.00 180.00 0.40 43 43 43 < 43 <0 so so so lunation i 3 MM o f 1 Mass f a i r ( ESP- ) In te r Channel Delay ( Seca I : Span ( D altons > : S t a r t T in a < Mina ) t End T ine { Mina ) : Repeats : Channel P aren t D aughter 0.03 0.00 0 .0 0 13.30 1 Dwell (Seca) C oll Energy (aVJ Cone ( v ) 1 421.00 0 .0 0 0 .4 0 40 00 L& V LAC. osL h fags 1 t*r 000598 BESTCOPYAVAILABLE jjk \ l tfa r M asslynx Sam ple List Sample List: C:\M ASSLYNX\rats2.PRO\Sam pleDB\031699b.SPL Printed: Tue M ar 1614:40:11 1999 ArUc DUW Page 1 File Nam e File Text MS File In let File 1 031699001 MeOH Blank PFO S-PFHS-IS long2 2 031699002 MeOH Blank PFO S-PFHS-IS long2 3 031699003 Tox120, R B L02229-H 2O B Ik-2,2/22/99 PFO S-PFHS-IS long2 4 031699004 Tox120, R B L02229-U vBlk-2,2/22/99 PFO S-PFHS-IS long2 5 031699005 TOX120, RBL02229-5ppb-2,2/22/99 PFO S-PFHS-IS long2 6 031699006 Tox120, RBL02229-1 Oppb-2,2/22/99 PFO S-PFHS-IS long2 7 031699007 Tox120, RBL02229-25ppb-2,2/22/99 PFO S-PFHS-IS long2 8 031699008 Tox120, RBL02229-50ppb-2,2/22/99 PFO S-PFHS-IS long2 9 031699009 Tox120, RBL02229-1OOppb-2, 2/22/99 PFO S-PFHS-IS long2 10 031699010 Tox120, R BL02229-250ppb-2,2/22/99 PFO S-PFHS-IS long2 11 031699011 Tox120, RBL02229-500ppb-2,2/22/99 PFO S-PFHS-IS long2 12 031699012 Tox120, R BL02229-750ppb-2,2/22/99 PFO S-PFHS-IS k>ng2 13 031699013 Tox120, RBL02229-1000ppb-2,2/22/99 PFO S-PFHS-IS long2 14 031699014 15 031699015 MeOH Blank T o x 1 2 0 ,1 6 1 F -G 5 ,2/22/99, d250 PFO S-PFHS-IS PFO S-PFHS-IS long2 long2 16 031699016 T o x120,162F -G 5,2/22/99, d250 PFO S-PFHS-IS long2 17 031699017 T o x120,163F -G 5,2/22/99, d250 PFO S-PFHS-IS long2 18 031699018 T o x120,164F -G 5,2/22/99, d250 PFO S-PFHS-IS k>ng2 19 031699019 T ox120,165F -G 5,2/22/99, d250 PFO S-PFHS-IS tong2 20 031699020 Tox120, RBL02229-250ppb-CC2,2/22/99 PFO S-PFHS-IS long2 21 031699021 MeOH Blank PFO S-PFHS-IS long2 22 31699022 Tox120,166F-G 5, 2/22/99, d250 PFO S-PFHS-IS long2 23 031699023 T o x120,167F -G 5,2/22/99, d250 PFO S-PFHS-IS long2 24 031699024 T o x120,168F -G 5,2/22/99, d250 PFO S-PFHS-IS long2 25 031699025 Tox120, RBL02229-250ppb-CC3,2/22/99 PFO S-PFHS-IS long2 26 031699026 MeOH Blank PFO S-PFHS-IS long2 27 031699027 T o x1 2 0 ,1 7 7 F -G 6 ,2/22/99, d1000 . PFO S-PFHS-IS long2 28 031699028 T ox120,1787F -G 6,2/22/99, d1000 PFO S-PFHS-IS long2 29 031699029 T o x120,179F -G 6,2/22/99, d1000 PFO S-PFHS-IS long2 30 031699030 T o x120,180F -G 6,2/22/99, d1000 PFO S-PFHS-IS long2 31 031699031 T o x120,181F -G 6,2/22/99, d1000 PFO S-PFHS-IS long2 32 031699032 Tox120, RBL02229-250ppb-CC4,2/22/99 PFO S-PFHS-IS long2 33 031699033 MeOH Blank PFO S-PFHS-IS long2 34 031699034 T ox120,182F -G 6,2/22/99, d1000 PFO S-PFHS-IS long2 35 031699035 T o x120,183F -G 6,2/22/99, d1000 PFO S-PFHS-IS long2 36 031699036 T o x120,184F -G 6,2/22/99, d1000 PFO S-PFHS-IS long2 37 031699037 T ox120,185F -G 6,2/22/99, d1000 PFO S-PFHS-IS long2 38 031699038 T ox120,186F -G 6,2/22/99, d1000 PFO S-PFHS-IS ' long2 39 031699039 Tox120, R BL02229-250ppb-CC5,2/22/99 PFO S-PFHS-IS long2 40 031699040 MeOH Blank PFO S-PFHS-IS long2 41 031699041 T ox120,187F -G 6,2/22/99, d1000 PFO S-PFHS-IS k>ng2 42 031699042 Tox120,169F-G Q , 2/22/99, d1000 P FO S -P FH S -IS . k>ng2 43 031699043 T o x120,190F -G 6,2/22/99, d1000 PFO S-PFHS-IS long2 44 031699044 T o x i2 0 ,191F -G 6 ,2/22/99, d1000 PFO S-PFHS-IS long2 45 031699045 Tox120, RBL02229-250ppb-CC6,2/22/99 PFO S-PFHS-IS long2 46 031699046 MeOH Blank PFO S-PFHS-IS long2 47 031699047 T o x1 2 0 .1 6 9 F -G 5 ,2/22/99 . PFO S-PFHS-IS long2 48 031699048 T ox120.170F -G 5,2/22/99 P FO S -P F H S -IS long2 49 031699049 T o x120.171F -G 5,2/22/99 PFO S-PFHS-IS long2 50 031699050 Tox120, RBL02229-250ppb-CC5, 2/22/99 PFO S-PFHS-IS long2 51 031699051 MeOH Blank P FO S -P F H S -IS long2 52 031699052 T ox120.173F -G 5,2/22/99 PFO S-PFHS-IS !ong2 53 031699053 T o x120.174F -G 5,2/22/99 PFO S-PFHS-IS long2 54 031699054 . T o x120.175F -G 5,2/22/99 PFO S-PFHS-IS long2 55 031699055 Tox120, RBL02229-250ppb-CC6,2/22/99 PFO S-PFHS-IS k>ng2 56 031699056 MeOH Blank PFO S-PFHS-IS long2 57 031699057 Tox120, RBL02229-H2O BIk-2,2/22/99 PFO S-PFHS-IS long2 58 031699058 Tox120, R BL02229-UvBlk-2,2/22/99 PFO S-PFHS-IS tong2 59 031699059 60 031699060 Tox120, R BL02229-5ppb-2,2/22/99 Tox120, RBL02229-10ppb-2,2/22/99 PFO S-PFHS-IS PFO S-PFHS-IS Iong2 long2 B ottle 91 91 1 2 3 4 5 6 7 8 9 10 11 91 12 13 14 15 16 82 91 17 18 19 83 92 20 21 22 23 24 84 92 25 ^ 26? 27 28 29 85 92 30 31 32 33 86 93 34 35 36 85 94 37 38 39 86 94 1 2 3 4 000S99 V olum e Sar 10 Ani 10 An: 10 Ani 10 An< 10 Sta 10 Sta 10 Sta 10 Sta 10 Sta 10 Sta 10 Sta 10 Sta . 10 Sta 10 Ani 10 Ani 10 Ani 10 Ani 10 Ani 10 Ani 10 QC 10 . Ani 10 An; 10 Ani 10 Ani 10 QC 10 An; 10 Ani 10 Ani 10 An; 10 An; 10 An 10 QC 10 An 1 0 : An 10 An 1 0 An 10 An 10 An 10 QC 10 An 10 An 10 An 10 An 10 An 10 Q( 10 At 10 Ar 10 Ar 10 Ar 10 Q< 10 Ar 10 Ar 10 Ar 10 Ar 10 Qi 10 Ar 10 Ai 10 Ar 10 SI 10 SI KSTCWmiUBlf b) 3 itef&9____ ;__________ ;____________ ______________ ;______ M asslynx - Sam ple List Sam ple List: C :\M ASSLYNX\rats2PRO \Sam pleDB\031699b.SPL Printed: Tue M ar 1614:40:11 1999 0L 2W Page 2 lA C P s/lolH F ile Nam e 61 031699061 62 031699062 63 031699063 64 031699064 65 031699065 66 031699066 67 031699067 F ile T ext TOX120, R B L02229-25ppb-2,2/22/99 Tox120, R B L02229-50ppb-2,2/22/99 Tox120, R B L02229-100ppb-2,2/22/99 Tox120, R B L02229-250ppb-2,2/22/99 Tox120, R B L02229-500ppb-2,2/22/99 Tox120, R BL02229-750ppb-2,2/22/99 Tox120, R B L02229-1000ppb-2,2/22/99 MS File P F O S -P F H S -IS P F O S -P F H S -IS P F O S -P FH S -IS P F O S -P FH S -IS PFO S-PFHS-IS P F O S -P FH S -IS P F O S -P FH S -IS In let File k>ng2 Ing2 long2 long2 long2 long2 long2 B ottle 5 6 7 8 9 10 11 Volum e Sai 10 Sta 10 Sta 10 Sta 10 Sta 10 Sta 10 Sta 10 Sta # I 000600 FACT: DATA REVIEW SUMMARY FORM Date: 3/nlqq Analyst: FACT Study Number AC, T o k -120 Matrix Time Points i d L L n/er fii-ppps. Gs-rm Dilutions? y * / * p - ----------- Analyte 1: UeJa)i'ttA Ibur Acceptable LinearRange: 1 LOQ far this data set: 9 1 m ---------- . Re-evahted fix differentrange? Alo Analyte 4: Acceptable Linear Range: LOQ for this data set: Re-evaluated for different range? Analyte 5: Acceptable Linear ] LOQ for this data set. Re-evaluatedfor differentrange? Analyte 6: Acceptable! anear Range: LOQ for thf< data set Re-evaluate*1for differentrange? Analyte 3: Acceptable Linear Range: LOQ for this data set . range? */ PFos t f Pfis Wtrt, in ietta tad stjJralti^. IC 0 3/!? /<}< } 1 . 000601 i s - I I I I t m nvnHMAAHA I H HH I SSSSSSSSSSlf SSSSiSSgSSSi 3 3 3 3 3 3 3 3 3 3 Z 3 3 3 3 3 o'ggggSSSSSSSSSgg gggSggggSgSgSggggSSSSgSaS S35SgSK Sggg2SS3?SSS K E E iS H |8H 3 E 3 3 g = = ||*||3 p i| | a S i||* H IS I ii S S U iU U s iE E S i l 3 H S H U H i S i I : s 3 i i S p s s s s p i p S S s S S j j p s ggggggggg gg ; "" 38855 . S S g g g g g Sgggggggg S 8 s s s "sssg'sss'j i l h h1 1 1 1 1 1 1 1 1 II 3 ' 5 5 i i ' ' a ' i . --3 : m S S S S S S S J S S S S S S SSSSii N O <> O O O TQ3CX20 R a t L i v a r G roup S an d < A m alia 062491 q u a n t i t a t a d a n d p r l n t a d e n 0 3 /1 7 /9 b y LAC J.J.H1 14 -- " " '' " " '' - " S S S S S S lS S S ia a s a S R g a S S R S S S R S S S S S S S S S S S S S S S S S G S S S S S S S S S G 8Q u a n t i f y C o m p o u n d t u m u r y B a p e r t 10X120 H at L iv e r G roup 8 and Saoplo L is t: G :\rata2.9ltt\6a4plaD B \031699b L a s t M o d ified : Hod Mar 17 13:54:10 1999 M othod: G :\rata2.P B 0\M ethD B \O 31699b L o o t a e d i f i o d : Wed Mar 17 0 8 :5 8 :2 0 159 Job Coda: P rinted: bod Mar 17 14:3 3 :5 8 1999 Cenpound 2 : f u r r 9 Mimo 1 031699001 2 031699002 3 031699003 4 031699004 5 031699005 6 031699006 7 031699007 8 031699008 9 031699009 10 031699010 11 031699011 12 031699012 13 031699013 14 031699014 15 031699015 16 031699016 17 031699017 18 031699019 19 031699019 20 031699020 21 031699021 22 031699022 23 031699023 24 031699024 25 031699025 26 031699026 27 031699027 28 03169902B 29 031699029 30 031699030 31 031699031 32 031699032 33 031699033 34 031699034 35 031699035 36 031699036 37 031699037 38 031699038 39 031699039 40 031699049 41 031699041 42 031699042 43 031699043 44 031699044 45 031699045 46 031699046 47 031699047 48 031699048 49 031699049 50 031699050 51 031699051 52 031699052 53 031699053 54 031699054 55 031699055 56 031699056 57 031699057 58 031699058 59 031699059 60 031699060 61 031699061 62 031699062 63 031699063 64 031699064 65 031699065 66 031699066 67 031699067 flaaplaliat la s t MaOH B lank KeOH B lank 7 o x l2 0 , RBL02229-R20Blk-2, 2 /2 2 /9 9 TOX120, RBL02229-IiivBlk-2, 2 /2 2 /9 9 7oxl20, RBL02229-5ppb-2, 2/22/99 Toxl20, RBL02229-10ppb-2, 2/2 2 /9 9 7oxl20, RBL02229-25ppb-2, 2/2 2 /9 9 Toxl20, *BL02229-50ppb-2, 2/22 /9 9 TOX120, *BL02229-100ppb-2, 2 /2 2 /9 9 10X120, *BL02229-250ppb-2, 2/22/99 T o x l2 0 ,` KBL02229-500ppb-2, 2 /2 2 /9 9 Toxl20, RBL02229-750ppb-2, 2 /2 2 /9 9 TOX120, RBL02229-1000ppb-2, 2 /2 2 /9 9 MeOK B lan k 1OX120, 161F-GS, 2 /2 2 /9 9 , d2S0 . 70X120, 162F-GS, 2 /2 2 /9 9 , 8250 70X120, 163IH35, 2 /2 2 /9 9 , d2S0 70X120, 164F-G5, 2 /2 2 /9 9 , d250 70X120, 165IW35, 2 /2 2 /9 9 , d250 7o x l2 0 , RBL02229-250ppb-CC2, 2 /2 2 /9 9 KaOH B lan k T o x l2 0 , lS r-G 5 , 2/22/99, d2S0 IOX120, 167P-GS, 2 /2 2 /9 9 , d2S0 TOX120, m r - C S , 2 /2 2 /9 9 , d2S0 TOX120, BBM2229-2S0ppb-CC3, 2 /2 2 /9 9 MaOH B lan k TOX120, m r - C i , 2 /2 2 /9 9 , dlOOO TOX120, n a / r - G S , 2/ 22/ 99, d io o o TOXI20, 179r-GC, 2 /2 2 /9 9 , dlOOO T0X120, l a o r - c s , 2/ 22/ 99, diooo TOXI20, OIF-GS, 2 /2 2 /9 9 , dlOOO TOXI20, RBL02229-2SOppfa-CC4, 2 /2 2 /9 9 MaOH B lank TOX120, 182r-GC, 2 /2 2 /9 9 , dlOOO TOX120, 183F-G. 2 /2 2 /9 9 , dlOOO TOX120, ltdF-GC, 2 /2 2 /9 9 , dlOOO TOX120, lOSr-G, 2 /2 2 /9 9 , dlOOO TOX120, 18SF-G6, 2 /2 2 /9 9 , dlOOO TOX120, BBL02229-250ppb-CCS, 2 /2 2 /9 9 MaOH B lank TOX120, 1871-G, 2 /2 2 /9 9 , dlOOO TOX120, 189F-G6, 2 /2 2 /9 9 , dlOOO T o x l2 0 , 190r-G 6, 2 /2 2 /9 9 , dlOOO T o x l2 0 , 191F-G, 2 /2 2 /9 9 , dlOOO TOX120, RBL02229-250ppb-CC6, 2 /2 2 /9 9 MaOH B lank TOX120. 189r-GS, 2 /2 2 /9 9 TOX120. 170r-G 5, 2 /2 2 /9 9 TO X l20.17lr-G S, 2/22/99 TOX120,' RBl02229-230ppb-CC5, 2 /2 2 /9 9 MaOH B lank TOX120. 1 7 3 M J , 2 /2 2 /9 9 TOX120. 174P-G5, 2 /2 2 /9 9 TOX120. 17C-GS, 2 /2 2 /9 9 TOX120, BBL02229-2S0ppb-CCC, 2 /2 2 /9 9 MaOH B lank TOX120, BBL02229~H20Blk-2, 2 /2 2 /9 9 TOX120, RBX,02229-LlvBlk~2, 2 /2 2 /9 9 Toxl20, BBL02229-Sppb-2, 2/2 2 /9 9 TOX120, RBL02229-10ppb-2, 2 /2 2 /9 9 ' TOX120, BBb02229-2Sppb-2, 2 /2 2 /9 9 TOX120, *BL02229-S0ppb-2, 2 /2 2 /9 9 TOX120, BBL02229-100ppb-2, 2 /2 2 /9 9 TOX120, ABb02229-250ppb-2, 2 /2 2 /9 9 TOX120, BBL02229-500ppb-2, 2 /2 2 /9 9 Toxl20, RBL02229-7S0ppb-2, 2 /2 2 /9 9 TOX120, RBL02229-1000ppb~2, 2 /2 2 /9 9 0 ^ > ix c o iH V i Vago 2 *VPA naly Analy A n aly A n aly S ta n d S ta n d S ta n d S ta n d S ta n d S ta n d S ta n d S ta n d S ta n d A naly naly A naly A n aly A naly A naly QC A n aly A n aly A n aly A naly QC A n aly A n aly A n aly A n aly A n aly A naly QC A naly A naly A n aly A n aly A n aly A n aly QC A n aly A naly A naly A naly A naly QC A naly 'A n aly A naly A naly QC A naly A naly A naly A naly QC A naly A naly A n aly S ta n d S ta n d S ta n d S ta n d S ta n d S ta n d S ta n d S ta n d S ta n d B td Cono ST 8.413 1.00 1.00 1.00 1.00 1.00 1.00 1 .0 0 1 .0 0 1.00 9.404 9.420 9.404 9.354 8.413 8.354 8.356 9.354 8.361 8.356 1 .0 0 8.290 6.379 8.453 1.00 8.37*9 6.384 8.384, 8.123 1.00 8.380 7.994 1.00 9.446 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1 .0 0 1.00 1.00 1.00 9.355 8.418 8.228 8.235 8.294 6.361 8.303 6.301 6.230 8.359 8.359 8.290 9.285 6.269 6.269 8.357 9.295 8.286 8.304 6.292 A rea 614 2274 2907 2500 2199 1931 . 2004 1623 1549 1775 48 12 737 7 1174 9 10 14 982 9 955 741 1213 601 617 809 1236 706 659 623 1229 1222 1139 . 1567 ^ 1317 1190 1278 1211 1102 1179 1136 Beaponae 684.42 2274.17 2906.68 2499.85 2189.27 1931.02 2004.23 1622.84 1548.69 1774.97 47.58 12.14 736.68 7 .0 6 1173.91 8.97 9.59 14.36 . 981.80 9 .1 5 955.41 Cono Tinga tCev 0.41 bb 1.37 bb 1.75 bb 1.51 bb 1.32 bb 1.16 bb 1.21 bb 0.98 bb 0.93 bb 1.07 bb 0.03 bb -59 37 75 51 32 16 21 -2 -7 7 -97 0.01 bb 0.44 bb 0.00 bb -99 -56 -100 0.71 bb 0.01 bb 0.01 bb 0.01 bb 0.59 bb 0.01 bb -29 -99 -99 -99 -41 -99 0.58 bb -42 740.87 1213.32 600.53 616.93 609.04 1235.83 706.35 657.72 623.03 1229.39 1221.94 1136.70 1567.05 1317.43 1169.57 1277.63 1211.23 1102.30 1178.91 1135.66 * % 0.45 bb 0.73 bb 0.36 bb 0.37 bb 0.49 bb 0.74 bb 0.43 bb 0.40 bb 0.38 bb 0.74 bb 0.74 bb 0.69 bb 0.94 bb 0.79 bb 0.72 bb 0.77 bb 0.73 bb 0.66 bb 0.71 bb 0.69 bb -55 -27 1 -64 -63 -51 -26 -57 -60 -62 -26 -26 -31 -6 -21 -28 -23 -27 -34 -29 -32 B a ta lla 0 6 2 4 9 * q u a n t i t a t a d a n d p r i n t e d o n 0 3 /1 7 /9 9 fey tA C 000603 Q u an tify C a lib ra tio n R ap o rt TCX12 0 1 s t L l v a r G r o u p 5 a n d * C a lib ra tio n : O :\rata2.pro\C urvuD B\031i99b L a a t a d l f l a d t Wad Mar 17 1 4 :3 7 :1 0 1*9 P rinted: Wad Mar 17 1 4 :3 4 :2 9 1999 y^g. , t o a l l a 0 4 2 4 9 9 q u a n t i t a t e d a n d p r i n t e d a n 0 3 /1 7 /9 9 b y 1AC 000604 Q n an tify C alib sa tio n X aport TOXI30 K a t U w G roup 5 a n d < C a llb ra tio n : G:\rm t* 2 .mo\CurvaDX\031(99b l a a t a o d i f i a d : a d Mas 17 1 4 )3 7 :1 0 19# P rlntad: a d Mar 17 14:34:3* 1**9 A m alla 04249* q o a n tlta ta d a n d p s ln ta d o a 0 3 /1 7 /9 9 b y U C 000605 Hacked apere 1 Method t i l e i La*t m odified: Oi \ r a t a 2 . PRO\KathDB\D31699b.mdb Nad H er 17 0 4 :3 4 :2 0 199 1 Confound Hama: Internal R at.: Q uantity Trace: Cone, o f Standard*: d o e r RP V a lu es 1 dear Peak Paccar: I n t e g r a t e Missdov f a c t o r s H09 [None] TIC Cone. X 1.000000, D isabled 1.000000 2 .0 0 0 R eten tio n Tiiae l a i u ) s R e la tiv e R e te n tio n Tima: Time Window (m in * ]: Peak Selections ] Reepenee Type: Raaponaa: 8 .45, Inablad 0.000. D iaabled 0.717 N earest S x te z n a l X reaa 1 Polynom ial Types Point o t O rigin: P it W eighting: xia Tran*form ation: L in ea r exclude 1/2 Hone 1 Unites Feak-to-pak am plituda: 293 S m oothing: Window s i a e t i c i a i ) : Humber o f sm ooths: Smoothing m sthod: D isablad 3 a Jo in v a lle y thrashold: Reduce paak ta ilin g : H a is b a a l in e maximum: ] Draw v e r t i c a l th r a a h o ld : D ataet shoulders: Shoulder th raah o ld : J R elativ h eig h t: A bsoluta height.: R elativ area: A bsoluta area: 30.00 70.00 4.00 10.00 D isablad 10.00 50. 00 Snablad 0.00 D isablad 3.00. B u b led 0.00 D isablad J ! 000606 Method Report M ethod f i l e s t e s t m o d ified : Compound: Printed: a :\rats2 .F R O \X eth D B \Q 3 1 f9 9 b .m d b N ed H er 17 0 < :3 6 ;2 0 1999 2: Surr Med Mer 17 12:11:29 1999 Coevound Mane: Internal Ret.: Quantify Trace: Cone, of Standards: Osar RP Value: Osar Peak Factor: Integrate Window Factor: Surr [Hone] TIC Fixed 1.000000, Disabled 1.000000 2.000 Retention Time (mins): Relative Retention Time: T i M Window (mins) s . Peak Selection: S.231, Enabled 0.000, Disabled 0.588 Nearest Response Typ: Response: External , ASM* polynomial Type: Point of Origin: Pit Weighting: Axis Transformation: Linear Exclude Hone None unit*! Paak-to-peak amplitude: 77 .Smoothing: Window aise <e*na): Humber of smooth*: Smoothing method: . Disabled 3 3 Join valley threshold: Reduce peek tailing: Raise baseline maximum: 30.00 70.00 4.00 Draw vertical threshold: Detect shoulders: Shoulder threshold: 10.00 Disabled 10.00 Relative height: Abaolute height: Relative area: ' Aheoluta area: 90.00. Enabled 0.00. Disabled 3.00, ttubled 0.00, Disabled AhL OUW lAc. mln-hl 000607 Q u a n tify Cengxnmd Sm xaaxy a p a rt TOX120 R a t U v a r O roup 9 a n d Saapl. U a t i S:\rata2.PHOMaaplaOB\03K99b L aat aodifiad: ad M ar 17 13:51:10 1999 Hathed: S:\rata3.m0\MathOB\O31999b3 L aat aodifiad: ad M ar 17 09:59:09 1999 Job Coda: Frintad: ad Mar 17 15:01:13 199 " n m m sm *8. 1 Compound Is FFB8 I Mima 1 031699001 2 031699002 3 031699003 4 031699004 3 031699005 6 031699006 7 031699007 03169900 9 031699009 10 031699010 11 031699011 12 031699012 13 031699013 14 031699014 15 031699015 16 031699016 17 031699017 1 03169901 19 031699019 20 031699020 21 031699021 22 031699022 23 031699023 24 031699024 25 031699025 26 031699026 27 031699027 28 031699028 29 031699029 30 031699030 31 031699031 32 031699032 33 031699033 34 031699034 35 031699035 36 031699036 37 031699037 38 031699038 39 031699039 40 031699040 41 031699041 42 031699042 43 031699043 44 031699044 45 031699045 46 031699046 47 031699047 4 031699049 49 031699049 50 031699050 51 031699051 52 031699052 53 031699053 54 031699054 55 031699055 56 031699056 57 031699057 58 031699058 59 031699059 60 031699060 61 031699061 62 031699062 63 031699063 64 031699064 65 031699065 66 031699066 67 031699067 G ? iac, aeplellet Text MtOK Blank KaOH Blank TOX120, RBL02229-B20Blk-2, 2/22/99 Toxl20, RBL02229-ItlvBlk-2, 2/22/99 TOX120, KBL02229-5ppb-2, 2/22/99 TOX120, *BL02229-10ppb-2, 2/22/99 TOX120, RBL02229-25ppb-2, 2/22/99 TOX120, *BL02229-50ppb-2, 2/22/99 TOX120, RBL02229-100ppb-2, 2/22/99 Toxl20, RBL02229-2S0ppb-2, 2/22/99 ?oxl20, RBL02229-500ppb-2, 2/22/99 TOX120, RBL02229-*750ppb-2/ 2/22/99' TOX120 RB102229-1000ppb-2, 2/22/99 HaOH Blank TOX120, 161F-G3, 2/22/99, d250 TOX120, 162FH55# 2/22/99, d250 Toxl20, 163F-GS, 2/22/99, d250 TOX120, 164F-GS, 2/22/99, d250 TOX120, 165F-G5, 2/22/99, d250 TOX120, *8102229-250ppb-CC2, 2/22/99 MaOK Blank TOX120, 166F-65, 2/22/99, d250 TOX120, 167F-GS, 2/22/99, d2S0 Toxl20, 168FHS5, 2/22/99, d250 70X120, BBL02229-2S0ppb-CC3, 2/22/99 HaOH Blank to TOX120, 1 7 7 M 6 , 2/22/99, dlOOO toxiio, naXr-G, 2/22/99, diooo Toxl20, 179r-CC, 2/22/99, diooo TOX120, 180F-C, 2/22/99, dlOOO 70X120, 181F-G, 2/22/99, dlOOO 7oxl20, BL02229-2S0ppb-CC4, 2/22/99 KaOH Blank 70X120, IB2F-G8, 2/22/99, dlOOO 10X120, 103F-GS, 2/22/99, dlOOO Toxl20, 1B4F-G6, 2/22/99, dlOOO Toxl20, 185F-G6, 2/22/99, dlOOO Toxl20, 18F-G6, 2/22/99, dlOOO 70X120, BL02229-250ppb-CCS, 2/22/99 HaOH Blank 70X120, 187F-GS, 2/22/99, dlOOO Toxl20, 199F-G6, 2/22/99, dlOOO Toxl20, 190F-G6, 2/22/99, dlOOO Toxl20, 191F-GS, 2/22/99, dlOOO 70X120, RBL02229-2S0ppb-CC6, 2/22/99 HaOH Blank 70X120. 1C9F-G5, 2 /2 2 /9 9 70X120. 170F-GS, 2 /2 2 /9 9 70X120. .171F-GS, 2/22/99 70X120, RBL02229-250ppb-CCS, 2/22/99 HaOH Blank 70X120. 173F-GS, 2/22/99 70X120. 174F-GS, 2/22/99 70X120. 17SF-G3, 2 /22/99 7oxl20, RBL02229-250ppb-CC(, 2/22/99 HaOH Blank 70X120, RBL02229-H20Blk-2, 2/22/99 7oxl20, RBL02229-LivBlk-2, 2/22/99 70X120, RBL02229-Sppb-2, 2/22/99 7oxl20, RBL02229-10ppb-2, 2/22/997oxl20, RBL02229-2Sppb-2, 2/22/99 70X120, BL02229-50ppb-2, 2/22/99 7oxl20, RBL02229-100ppb>2, 2/22/99 70X120, BBLO2229-2S0ppb-2, 2/22/99 7oxl20, RBC02229-500ppb-2, 2/22/99 70X120, BBL02229-7S0ppb-2, 2/22/99 70X120, RBL02229-1000ppb-2, 2/22/99 Typa . Bnaly Bnaly Bnaly Bnaly Stand Stand Stand Stand Stand Stand Stand Stand Stand Bnaly Bnaly Bnaly Bnaly Bnaly Bnaly QC Bnaly Bnaly Bnaly Bnaly QC Bnaly Bnaly Bnaly Bnaly Bnaly Bnaly QC Bnaly Bnaly Bnaly Bnaly Bnaly Bnaly QC' Bnaly Bnaly Bnaly Bnaly Bnaly QC Bnaly Bnaly Bnaly Bnaly QC Bnaly Bnaly Bnaly Bnaly QC Bnaly Bnaly Bnaly Stand Stand Stand Stand Stand 'Stand Stand Stand Stand ltd Ceno XT 5.99 12.00 29.90 59.90 120.00 299.00 599.00 898.00 1198.00 7.878 7.829 7.812 7.828 7.820 7.826 7.830 7.826 7.832 299.00 7.830 7.893 7.849 7.901 7.889 7.850 299.00 7.857 7.793 7.857 7.850 299.00 7.849 299.00 7.851 299.00 299.00 299.00 7.827 7.889 7.766 7.770 7.702 7.831 7.775 7.711 7.765 5.99 12.00 29.90 59.90 120.00 299.00 599.00 98.00 1198.00 7.761 7.757 7.762 7.763 7.766 7.770 7.759 7.775 7.766 Area 52 93 216 325 751 1966 3677 5126 7909 2007 2569 2200 2150 2715 2299 2120 2652 1786 2773 1980 2185 2065 2303 999 1350 1319 234 175 203 1298 46 99 . x 178 328 730 1710 3403 5157 7163 Itaa p o n a Ceno. Fla. tCav 51.87 92.97 216.31 325.31 750.60 1965.87 3676.73 5125.94 7909.42 2007.43 2569.44 2199.84 2149.83 2714.90 2299.14 2120.11 2651.97 1785.69 *2772.88 5.86 bb 12.91 HM 34.09 MM 52.81 bb '125.83 bb 334.50 bb 628.26 bb 77.10 bb 1355.04 bbX 341.64 MM 438.13 KM 374.67 KM 366.09 MM 463.11 MM 391.72 bb 360.98 MM 452.31 MM 303.56 MM 473.07 MM -2 8 14 -12 5 12 5 -2 13 31 i 58 1979.57 338.95 bb 13 2184.78 372.08 bb 24 2064.91 2303.09 998.60 1350.47 1319.16 233.79 175.09 202.65 1298.25 351.50 MM 392.40 bb 168.41 bb : 228.83 MM 223.45 bb 37.09 bb 27.01 MM 31.74 bb 219.86 bb 18 * -25 -2 fi- 46.35 98.73 177.97 328.19 730.44 1709.98 3402.77 5157.15 7163.23 . 4.91 MM 13.90 bb 27.51 MM 53.30 MM 122.37 MM 290.56 MM 581.22 MM 882.46 MH 1226.91 bbX -18 16 -8 -11 2 -3 -3 -2 2 Cal, Cktck-i fr- * 3 tvtrt, outierj, wUt &}l oHur c-c ixftrc WiUv'V. C-rilcrO. CaL ChicJo will W u A o - H u r j In d a V a $t,V- Vo v & r ^ uktjlur or n-V *Vk,j daVa. 3 ac.ttjiVfttile. H e o iln h j ftrt ouin. TP Con(V/'c/ ucs 3 -,1o Vtonu. . t f U f c l W W j k A m a l i a 0 6 2 4 9 8 : q u a n t i t a t a d a n d p r i n t a d e n 0 3 / 1 7 / 9 9 b y LAC 000608 cW rJ Mi 3, Q u a n tify CoBpeond S u n eary S taport 10X120 H at l i v a r G roup S and C 8ampia List: G:\rata2.P90\5aqpleDB\O31699b Lait modifiad: ed far 1? 13:54:10 1999 Mnthod: G : \ r a t s 2 .PR0\>4athDB\O31699b2 Laat nodlfied: Wed Mar 17 04:39:09 1999 Job Ceda: Printed: ad Mar 17 15:01:13 1999 Coapound 2 : Surr ama 1 031699001 2 031699002 3 031699003 4 031699004 & 031699005 4 031699006 7 031699007 t 031699008 9 031699009 10 031699010 11 031699011 12 031699012 13 031699013 14 031699014 13 031699015 14 031699016 17 031699017 14 031699016 19 031699019 20 031699020 21 031699021 22 031699022 23 031699023 24 031699024 25 031699025 24 031699026 27 031699027 29 031699028 29 031699029 30 031699030 31 031699031 32 031699032 33 031699033 34 031699034 35 031699035 34 031699036 37 031699037 38 031699038 39 031699039 40 031699040 41 031699041 42 031699042 43 031699043 44 031699044 45 031699045 46 031699046 47 031699047 48 031699048 49 031699049 50 031699050 SI 031699051 52 031699052 53 031699053 54 031699054 55 031699055 56 031699056 * 57 031699057 58 031699058 59 031699059 60 031699060 61 031699061 62 031699062 63 031699063 64 031699064 65 031699065 66 031699066 67 031699067 S a a p l a U a t Tmxt M*OK Blank M.0H Blank Toxl20, RBL02229-H20Blk-2, 2/22/99 Toxl20, ftB1.02229-UTBlk-2, 2/22/99 Ioxl20, m02229 - S p p b - 2 , 2/22/99 TOX120, RBL02229-10ppb-2, 2/22/99 TOX120, BBL02229-25ppb-2, 2/22/99 TOX120, BBt,02229-S0ppb-2. 2/22/99 Toxl20, BBL02229-l00ppb-2, 2/22/99 Toxl20, RBL02229-250ppb-2, 2/22/99 Toxl20,-ULa2229-900ppb-2, 2/22/99 TOX120, BBL02229-7S0ppb-2, 2/22/99 TOX120, BBLG2229-- 1000ppb*>2, 2/22/99 ttaOB Blank 70X120, 1S1F-G3, 2/22/99, d2S0 70X120, 1C2F-GS, 2/22/99, d2S0 ' 70X120, 163F-G5, 2/22/99, d2S0 7OX120, l4r-S, 2/22/99, <1290 70X120, ICSr-GS, 2/22/99, d290 70X120, RBL02229-2S0ppb-CC2, 2/22/99 XaOH Blank 7oxl20, 1SSF-G5, 2/22/99, d230 70X120, 1S7F-6S, 2/22/99, <1230 70X120, 168F-G5, 2/22/99, <1230 70X120, RBL02229-230ppb-CC3, 2/22/99 MaOH Blank A 70X120, 177F-GS, 2/22/99, dlOOO 70x120, m i r - c i , 2/22/99, diooo TOX120, 179F-G6, 2/22/99, dlOOO 70X120, 180F-G6, 2/22/99, dlOOO 70X120, 181F-G8, 2/22/99, dlOOO 70X120, BBli02229~250ppb-- CC4, 2/22/99 HaOH Blank 70X120, 182F-G8, 2/22/99, dlOOO 70X120, 183F-G6, 2/22/99, dlOOO TOX120, 194F-G4, 2/22/99, dlOOO 70X120, 183F-G, 2/22/99, dlOOO TOX120, 188F-64, 2/22/99, dlOOO Toxl20, RBl02229-250ppb-CC5, 2/22/99 KaOK Blank 70X120, 187F-GS, 2/22/99, dlOOO 70X120, 189F-G6, 2/22/99, dlOOO 70X120, 190r-G6, 2/22/99, dlOOO 70X120, 191F-G8, 2/22/99, dlOOO 70X120, RBU32229-250ppb-CC6, 2/22/99 KaOB Blank 70X120. 169F-GS, 2/22/99 70X120. 1 7 0 M S , 2/22/99 70X120. 171F-G5, 2/22/99 70x120, BBL02229-230ppb-CCS, 2/22/99 HtOU Blank 70X120. 173F-GS, 2/22/99 70x120. 174F-GS, 2/22/99 7oxl20. 17SI^GS, 2/22/99 70X120, RBU)2229-250ppb-CC<, 2/22/99 HaOH Blank 7oxl20, m02229-H2OBlk-2, 2/22/99 70X120, BBt.02229-LiaBlk-2, 2/22/99 7oxl20, RBL02229-5ppb-2, 2/22/99 70X120, RBU)2229-10ppb-2, 2/22/99 7oxl20, BBL02229-2Sppb-2, 2/22/99 7oxl20, BBli02229-30ppb*2, 2/22/99 70X120, BBl*02229-100ppb*2, 2/22/99 7oxl20, BB1.02229-23appb-2, 2/22/99 7oxl20, BB02229-500ppb-2, 2/22/99 70X120, Bt.02229-7S0ppb-2, 2/22/99 70X120, BB1.02229-10aOppb-2, 2/22/99 (f > @ IA C 03 Typo taaly Bnaly Analy Bnaly Stand Stand Stand Stand Stand Stand Stand Stand Stand Bnaly Bnaly Bnaly Bnaly Bnaly' Bnaly OC Bnaly Bnaly Bnaly Bonca l y Bnaly Bnaly Bnaly Bnaly Bnaly Bnaly OC Bnaly Bnaly Bnaly Bnaly Bnaly Bnaly . oc Bnaly Bnaly Bnaly Bnaly Bnaly. oc Bnaly Bnaly Bnaly Bnaly OC - Bnaly Bnaly Bnaly Bnaly OC Bnaly Bnaly Bnaly Stand .Stand Stand Stand stand Stand Stand Stand Stand . Std Cena xr 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.412 8.482 8.404 8.420 8.404 8.354 8.413 8.354 8.358 8.354 8.361 6.356 1.00 8.290 6.378 8.453 1.00 8.379 6.364 8.384 6.123 1.00 8.380 7.9B4 1.00 8.446 1.00 8.355 * 8.418 8.228 6.235 1.00 8.294 1.00 8.361 8.303 8.301 8.230 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 8.359 6.359 8.290 8.285 8.269 8.289 8.357 8.295 6.286 6.304 8.292 Area 684 904 2274 2907 2500 2189 1931 2004 1623 1549 1775 48 12 737 7 1174 9 10 14 982 9 955 . 741 1213 601 617 809 1236 706 658 623 1229 1222 1139 1567 1317 1190 1278 1211 1102 1179 1136 Aeapona 684.42 903.69 2274.17 2906.68 2499.85 2189.27 1931.02 2004.23 . 1622.84 1548.68 1774.97 47.56 12.14 736.68 7.06 * 1173.91 8.97 9.59 14.36 981.80 9.15 955.41 Cono. Fina. .Dm 0.41 bb 0.54 bb 1.37 bb 1.75 bb 1.51 bb 1.32 bb 1.16 bb 1.21 bb 0.96 bb 0.93 bb 1.07 bb 0.03 bb -59 -46 37 75 SI 32 16 21 -2 -7 7 -97 0.01 bb 0.44 bb 0.00 bb -99 -56 -100 0.71 bb 0.01 bb 0.01 bb 0.01 bb -29 -99 -99 -99 0.59 bb - -41 0.01 bb -99 0.58 bb -42 740.97 0.45 bb 1213.32 600.53 616.93 809.04 1235.83 706.35 - 657.72 623.03 : *i * 0.73 bb 0.36 bb 0.37 bb 0.49 bb 0.74 bb 0.43 bb 0.40 bb 0.38 bb 1229.39 1221.94 1138.70 1567.05 . 1317.43 1189.57 1277.63 1211.23 1102.30 1178.81 1135.66 0.74 bb 0.74 bb 0.69 bb 0.94 bb 0.79 bb 0.72 bb 0.77 bb 0.73 bb 0.66 bb 0.71 bb 0.68 bb -55 -27 -64 -63 -SI -26 -57 -60 -62 -26 -26 -31 -6 -21 -28 -23 -27 -34 -29 -32 A m alia 0 4 2 4 9 9 : q u m n tita ta d a n d p r i n t a d m i 0 3 /1 7 /9 9 k y IAC 000609 Q u an tify C a lib ra tio n K ap ert 100(120 R a t L i v a r G ro u p 9 a n d ( Calibratieni a : \ r a t a 2 . P m \CurmDB\03M99b2 Last modified: Wed Mar IT 19:09:90 1**9 Printed: Wad Ma r 17 19:01:49 199* Pag 1 000610 Q u a n tify C a lib ra tio n R ap o rt TQX120 R a t L l v a r C ro u p S a n d 3 Calibration: a:\rata2.3RO\CurraOB\031l93ba Laat nodifiad: Wad Mar 17 18:04:30 1333 prlntad: Wad Mar 17 13:01:43 ! fW 2 I n a i l a 062498: q uant i t a ra d and p r ln ta d on 0 3 /1 7 /3 3 b y M C 000611 1 Method Report Method file: 1 Last modified: Compound: printed: O:\rats2.FRO\MethDS\031699b2.ndb Wa d Mar 17 06:39:09 1999 1: FFHS W ad Mar 17 1 3 : U : 3 S 1999 1 Compound Mane: Internal Ref.: Quantify Trace: Cone, of Standards: u*c r f valuei I User Pm I Factor! Integrate Window Factor t **** , ,n 3 9 9 . 0 0 00.00 Cone. * 1.000000, Disabled 1.000000 2.000 tetnfcioa T i M (lint) i 1 Relative Retention Tim*: T i M Window (mine) t Peak Selection: 7.543, Xnablod 0.000# Disabled 0.020 XMTMt Response Typo i ] Response: eternal Arons polynomial Typ* 1 Point of Origin: Pit weighting: Axia Transformation: Exclude 1/X 1 units: Peak-to-peak amplitude: Window eixe (scans): Number of smooths: Smoothing method; 293 Dlaablad J * J oin valley fehraahoid: * Jtadoca peak tailing: Raise baseline auxiaum: 30.00 70.00 4.00 Draw vortical threshold: Datact shoulders: Shoulder threshold: / 10.00 Disabled 10.00 J Relative height! Absolute height: Relative are.: Rbaolute area: 50.00, Snabled 0.00, Disabled 3.00, Enabled 0.00, Disabled ! Artekd 0LW8________/AC Qllfrlw j: I 000612 M ethod R e p o rt H ath o d f i l e : L u t B O d lfiad : Confound: P rin te d : O :\r.ta2 .F R O \H eth L B \0 3 1 i9 9 b 2 .sd b Wad W ar 17 0 i:5 S :0 J 1599 2 : Surr Wed M u 1 7 1 3 :1 1 :3 3 1991 Conpouad Naaei Internal Ret.t Quantity Trace: Cone, of 3tenderda: Bear RF Value: D a n Peek Factor: Integrate Window Factors Sun (Hone) TIC Fined 1.000000, Disabled 1.000000 2.000 Retention Tine (mine) i Relative Retention Tine: Tine Window (nine) t Peek Selection: 9.331, Rnabled 0.000, Disabled o.saa Nearest Response Type: Responses Brterael Areas Polynomial Types Point of Origin: Fit Weighting: Axis Transformations Linear Ktclude Hon Hone Units; Feak-to-peak amplitude: Smoothing: Window site (scans): Humber of smoothes Smoothing methods 77 Disabled 3 2 Join valley thresholds ` Reduce peak tailings Raise baseline maximum: 30.00 70.00 4.00 Draw vertical threshold; Detect ehouldere: Shoulder thresholds 10.00 Disabled 10.00 Relative heights Absolute heights Relative areas . Absolute areas SO .00,, Bnahled . O.OOg Disabled 3.00. enabled 0.00. Disabled A tJ ia . o m w ____ AC__ 000613 FACT: DATA REVIEW SUMMARY FORM Date: * /s h i 000614 Q u an tify Conpound Susaaxy R eport Tox-120 R a t U v u Raspi* U s t i M:\rata2.PRO\aasplaDa\04209Ra Last nodlflad: Thu Apr 22 09:02:11 1999 Method: H:\rats2.9R0\ttethDB\042099o Last nodlflad: Tu* May 04 08:52:41 1999 Job Cod*: Printed: Hod May OS 11:10:51 1999 BESFcopyAMliABIE Pag* 1 Compound 1: PQAA Sanplallat Taxt Typ Std Conn XT Arra Xaapona Cene. llaga 4Dv 042099002 MsOM Blank 042099003 042099004 042099005 04209900 042099007 042099008 042099009 042099010 10 042099011 11 042099012 12 042099013 TOX120, RBL04199-H20Blk-l, 4/19/99 TOX120, RBL04199-UTBlk-l, 4/19/99 Toxl20, RBL041S9*3ppb-l. 4/19/99 TOX120. RBL04199-10ppb-l, 4/19/99 TOX120, RBL04199-25ppb-l, 4/19/99 TOX120, RaL04199-50ppb-l. 4/19/99 TOX120, ABL04199-100ppb-l, 4/19/99 TOX120, RBL04199-250ppb>l, 4/19/99 Toxl20, BBL04199-S00ppb-1, 4/19/99 Toxl20, RBL04199-750ppb-l, 4/19/99 TOX120, RBL04199-1000ppb-l. 4/19/99 Standard Standard Standard . Standard Standard Standard Standard Standard . Standard 5.56 11.10 27.80 55.60 111.00 278.00 556.00 833.00 1111.00 4.483 4.480 4.477 4.479 4.479 4.486 4.484 4.481 4.484 74 37 77 121 16S 374 140 922 107S 73.837 57.350 76.531 121.096 165.361 374.157 739.533 921.621 1074.679 32.81 MM . 20.70 HM 34.85 MM 7.75 MM 100.42 bb 254.53 bb 524.21 MM <58.0 bbX 771.72 bbX 86 25 22 -10 -8 -6 -21 -31 13 042099014 HOH Blank 14 042099015 Toxl20, RTL, IM, Gl, 4/19/99 15 042099016 16 042099017 OX120, RTL, 2M, Gl, 4/19/99 ToxllO, RTL, 3M, Gl, 4/19/99 17 042099018 TOXI20, RTL, 4M, Gl, 4/19/99 16 042099019 19 042099020 TOXI20, RTL, SH, Gl, 4/19/99 T0XI20, RBL04199-250ppb~CCl, 4/19/99 QC 278.00 4.483 355 354.906 240.32 bb 20 042099021 HaOH Blank 21 042099022 T0XI2O, RTL, M, Gl, 4/19/99 22 042099023 TOXI20, RTL, TM, 61. 4/19/99 23 042099024 TOXI20, RTL, SM, Gl, 4/19/99 24 042099025 TOXI20, RTL, 9M, Gl, 4/19/99 25 042099026 26 042099027 TOXI20, RTL, 10H, Gl, 4/19/99 T0XI2O, RBL04199-250ppb-CC2, 4/19/99 OC 278.00 4.480 447 447.316 308.53 bb 11 27 042099028 28 042099029 MaOH Blank T0XI2O, RTL, U M , Gl, 4/19/99 29 042099030 T0XI2 O, RTL, IBM, Gl, 4/19/99 30 042099031 T0XI2O, RTL, 14M, Gl, 4/19/99 31 042099032 32 042099033 T0XI2O, RTL, 15M, Gl, 4/19/99 T0XI2O, RBL04199-250ppb-CCl, 4/19/99 oc 278.00 4.484 341 341.490 230.42 MH 33 042099034 MaOH Blank 34 04209903S TOXI20, RTL, 17K, G2, 4/19/99 35 042099036 TOXI20, RTL, 18M, G2, 4/19/99 36 042099037 TOX120, RTL, 19M, G2, 4/19/99 37 042099038 TOXI20, RTL, 2OM, G2, 4/19/99 38 042099039 TOXI20, RTL, 21M, G2, 4/19/99 39 042099040 TOXI20, RBL04199-2J0ppb-CC4, 4/19/99 40 042099041 MaOH Blank 41 042099042 TOX120, RTL, 22M, G2, 4/19/99 42 042099043 T0XI2 O, RTL, 23M, G2, 4/19/99 43 042099044 TOXI20, RTL, 24M, 62, 4/19/99 44 042099045 TOXI20, RTL, 2 SM, G2, 4/19/99 45 042099046 TOXI20, RTL. 2 SM, G2, 4/19/99 46 042099047 TOXI20, RBL04199-2S0pph-CC5, 4/19/99 QC QC 278.00 4*480 4.482 4.480 4.471 4.495 4.47 3899 5143 5371 5320 5764 413 4.479 4423 4.479 3922 4.487 5424 4.485 2795 4.484 3068 278.00 4.479 343 3898.674 5142.572 5371.353 5319.678 5764.340 413.054 2855.93 bb 3774.03 bb 3942.89 bb 3904.90 bb 4232.95 bb 283.24 bb 4422.820 3922.058 5424.250 2794.636 3067.762 342.693 3242.79 bb 2873.19 bb 3981.94 bb 2041.05 bb 2242.64 bb 231.30 MH fO-to, I ' I S d ilu W 47 042099048 MaOH Blank 4*8 042099049 TOXI20, RTL, 27M, 62, 4/19/99 49 042099050 T0XI2O, RTL, 29M, 62, 4/19/99 J 50 042099051 51 042099052 52 042099053 53 042099054 54 042099055 TX120, RTL, 3OM, G2, 4/19/99 T0XI20, RTL, 31M, 62, 4/19/99 TOXI20, RBL04199-250ppb-CC, 4/19/99 MaOH Blank T0XI2O, RTL, 33M, 63, 4/19/99 QC 55 042099056 T0XI2 O/ RTL, 34M, 63, 4/19/99 56 042099057 TOXI29, RTL, 3SM, G3, 4/19/99 57 042099058 TOXI20, RTL, 36M.'63, 4/19/99 58 042099059 TOXI20, RTL, 37M, G3, 4/19/99 59 042099060 TOXI20, RBL04199-250ppb-CC7, 4/19/99 QC 278.00 278.00 4.484 4.483 4.479 4.479 4.483 4.481 4.479 4.479 4.495 4.453 4.495 2119 1448 1545 1644 419 4232 5668 4583 4657 5081 411 2119.342 1448.030 1544.621 1644.361 418.663 1542.63 bb 1047.14 bb 1118.43 bb 1192.05 bb 287.38 bb 4232.225 5668.119 4582.970 4657.182 5081.245 411.447 3102.12 bb 4161.93 bb 3361.00 bb 3415.77 bb 3728.77 bb 282.05 MM ^ bitA l*lo U 60 042099061 61 042099062 62 042099063 63 042099064 64 042099065 65 042099066 66 042099067 MaOH Blank 4 TOXI20, RTL, 38M, 63, 4/19/99 TOX120, RTL, 39M, 63. 4/19/99 T0XI2O, RTL, 4OM, 63, 4/19/99 ' TOX120, RTL. 41M, G3, 4/19/99 TOX120', RTL, 42M, 63, 4/19/99 TOXI20, RBL04199-250ppb-CC8, 4/19/99 QC 278.00 4.472 .4*483 4.475 4.488 4.481 4.480 5831 4587' 5604 . 3410 1319 443 5631.017 4587.398 5603.629 3409.806 1318.606 442.641 4134.55 MM 3364.27 IM 4114.33 bb 2495.10 bb 951.61 bb 305.07 bb 67 042099068 68 042099069 69 042099070 70 042099071 71 042099072 `72 042099073 MaOH Blank T0XI2O. RTL, 43M, 63, 4/19/99 TOXI20, RTL, 45H, 63, 4/19/99 TOX120, RTL, 4EM, G3, 4/19/99 TOXI20, RTL, 47M, G3, 4/19/99 TOXI20, RBL04199-250ppb-CC9, 4/19/99 QC 278.00 4.483 4.479 4.480 4.486 4.484 2595 1076 650 1384 398 2594.520 1075.927 850.322 1383.690 398.107 1893.35 bb 772.50 bb 605.99 bb 999.65 bb 272.20 MM 73 042099074 MaOH Blank 74 04209907 TOX120, RTL, 5M, 05, 4/19/99 75 04209907 TOX120, RTL. 6M. 05, 4/19/99 7 042099077 TOX120, RTL, 73H, 05, 4/19/99 ' 77 04209907 TOX120, RTL. 74M, 05, 4/19/99 78 042099079 79 042099080 80 042099081 TOX120, RTL, 7SM, GS, 4/19/99- TOX120, R9L04199-250ppb-CC4, 4/19/99 MaOH Blank OC 278.00 4.454 413 413.360 283.48 MM 81 042099082 TOX120. RTL, 77H, 05, 4/19/99 82 042099083 TOX120, RTL, 78M, GS, 4/19/99 83 042099084 84 042099085 Toxl20, RTL, 79M, OS, 4/19/99 TOX120, RBL04l99-2S0ppb-CCS, 4/19/99 QC 278.00 4.459 364 363.646 246.77 W 85 04209908 86 042099087 87 042099088 88 042099089 MaOH Blank TOX120, RTL, 3M, Gl-2S0ppb-H3, 4/19/99 Toxl20, RTL, 3H. Gl-2S0ppb-MSD, 4/19/99 TOX120, RTL, CM. Ql-2S0ppb-MS, 4/19/99 4.477 4.472 4.485 372 372.063 252.98 bb 380 360.105 258.92 MM 385 384.795 262.38 bb ,m ad elin * 041099: q u a n tita ta d and p r ln ta d by i 5 /0 9 /9 9 000615 1 1 ! ] Quantify Compound Summary Raport Tox-120 Rat U v Saapla U a t : N:\zata2.PRO\8amplaDB\04209Sa last modlflads Thu Apr 22 09:02:11 1999 Hathod: H:\rata2.PRO\MathDB\042099a Last modlflad: Tua Hay 04 09:52:4 1999 Job Coda: Printad: ad Hay 05 11:10:51 1999 Compound 1: PGAA 1 Mu m 89 042099090 90 042099091 91 042099092 92 042099093 93 042099094 94 042099095 95 042099096 96 04209909*7 9*7 042099099 98 042099099 99 042099100 100 042099101 101 042099102 102 042099103 103 042099104 104 04209910S Samplallat Tax Typ fltd Cono TSX120, RTL, 6H( Gl-2S0ppb-M3D. 4/19/55 T0X120, RTL, 13H, 61-250ppb-HS, 4/19/99 TOX120, RTL, 13H, Gl-2iOppb-HSO, 4/19/99 Toxl20, RBL04199-250ppb-CC6, 4/19/99 OC 278.00 H*OK Blank ToxllO, RBL04199-H20BU-1, 4/19/99 Toxl20, R8L04199-LlvBlk-l, 4/19/99 TOX120, RBL04199-Sppb-l, 4/19/99 Toxl2( RBL04199-10ppb-l, 4/19/99 Toxl20, RBL04199-25ppb-l, 4/19/99 Toxl-20, RBL04199-50ppb-l, 4/19/99 TOX120, RBL04199*100ppb-l, 4/19/99 TOX120, RBL04199-250ppb-l, 4/19/99 TOX120, R8L04199-S00ppb-1, 4/19/99 TOX120, RBL04199-750ppb-l, 4/19/99 Toxl20, RBL04199-1000ppb-l,'4/19/99 Standard Standard Standard Standard . Standard Standard Standard Standard Standard 5.5 11.10 27.80 55.60 111.00 278.00 556.00 833.00 1111.00 XT 4.483 4.484 4.486 4.475 4.485 4.479 4.484 4.483 4.483 4.484 4.470 4.485 4.484 4.441 hgt 2 Aru 397 492 449 377 110 18 57 89 107 173 381 847 1080 1247 Xaipon 397.088 492.434 449.098 376.897 Cone. Flogs %Dev 271.45 bb 341.83 bb 309.84 bb 256.55 MM -8 110.250 17.853 56.918 8.793 107.191 172.713 380.632 647.164 1080.222 1247.489 59.74 bb 0.00 MM 20.38 bb 43.90 MM 57.48 bb 105.84 bb 259.31 bb 603.65 MM 775.67 MMX 899.12 bbX -100 84 56 3 -5 -7 9 -7 -19 j 1 ] ! i r m ad alln a 041099: :q u a n tlta ta d and p r in ta d by m aa 5 /0 5 /9 9 i is 000616 I g ssssassssa ssaass sssssn sascs ssgasa ssssss aaass ssssss ssasss assss ssaasa sssssass s i i s ia - " - s a l a s s a i i i i H s s s s r s g a s s a i i i i i i s a s a s s i v i ss.ssg sg asa a s s s S t r i s i I ssssasssa saageS ssaasii salsa aaaali sass-s sasis sasssa sassss assss ssSsss sSsalsas 3HSSS5Sg H H H P 'i i i2 | 333SS MU U U U t t i i SSISss alias issasi S5S58|s | J SHSaasSsas S58gg ffil iliS a SaSSI saassl salsa 4SS3!'E>333g SSSSg S3g33g &g' ggg s ssssaassss saassa sSaass sassi sasasa aassia ssaas saasss aiassa sassi sassi? aasssaas l 52S8SSSSS s ss i 5 s s s g s ss m N b illi [lp (afa [sfa' ]s s ^s m S s3 a s a s 1 2 \ li..I| 1filai sIg s -J'T . s- m i r | S3SS; s'ssss .s8s8'8s'8s8sSs s3'3s'3s3's3's1's 3`8'88'f 833*33 s's's'ss"^ 33331 SSBBsf 3SS5. ggg i --ssssssti m Y ii m t i l * * & i i i i i m M i i m i i U m i i i i i t t i t t m m i m > g g o g g g g g g g S o 0*0=o a o'o'o 0 =0800 o o o 3 00 0*000 a 00 00 00 a 00000S g o'o'o'o oSoo'o'o o o 3 g-g'g'g'g-agg'g'gg'g a gg-g-g-a g gg ' pgwgggo^NM^*nr^a>OjjjNrn inv^wre [U H I! l i s ils iiiis s iiis s s s s s s s s s s is s s is is is s s sIissHiiSss s; is s s s s is iiiis s lis s s s lillig s s ls s s s llis ii; wr--sasnsssasssasasasRsssasasasKssgasaasaaaasaaasasKsssassasscsssaspsssssssasssssss Q u a n t if y C om pound Suom iary R a p o r t Tox-120 R at U v a r Sampla Liat: H:\rata2.PR0\SamplaDB\042099o l u t modifiad: Thu Apr 22 09:02:11 1999 Mathod: M:\rata2.P9O\MathDB\042099c Laat modifiad: Tua May 04 09:92:49 1999 Job Coda: Printad: Wad May 09 11:10:91 1999 BESTCOPY AVAILABLE Pacja 4 Compound 2: 9109 9 Mama 09 042099090 90 042099091 91 042099092 92 042099093 93 042099094 94 042099095 95 042099096 96 042099097 97 042099099 90 042099099 99 042099100 100 042099101 101 042099102 102 042099103 103 042099104 104 042099105 Samplaliat Text * Toxl20, m , 6M. Gl-2S0ppb-MSD, 4/19/99 Std Cena TOX120, RTL. 13M. Gl-2S0ppb-M3, 4/19/99 TOX120, RT1, 13M, Gl-250ppb-H3D, 4/19/99 TOX120, RBL04199-250ppb-CC6, 4/19/99 QC 279.00 MaOH Blank Toxl20, RBL04199-H2OBU-1, 4/19/99 Toxl20, RBL04199-UvBlk-l, 4/19/99 Toxl20, RBL04199-5ppb-l, 4/19/99 Toxl20, BBL04199-10ppb-l, 4/19/99 Toxl20, RBL04199-25ppb-l, 4/19/99 TOX120, RBL04199-S0ppb-1, 4/19/99 Toxl20, RBL04199-100ppb-l, 4/19/99 ToxI20. *BL04l99-250ppb-l, 4/19/99 TOX120, RBL04199-S00ppb-1, 4/19/99 TOX20, RBL04199--750ppb~l* 4/19/99 TOX120, RBL04199-1000ppb-l'.' 4/19/99 Standard Standard Standard Standard Standard Standard Standard Standard Standard 5.56 11.10 27.80 55.60 111.00 278.00 556.00 033.00 1111.00- RT 4.622 4.779 4.760 4.616 4.924 4.760 4.619 4.760 4.776 4.779 4.776 4.906 4.779 4.779 4.760 Arsa 2997 2906 2923 2396 57 139 164 199 382 637 1056 2337 4350 6492 7651 Raapanaa 2987.061 2905.830 2922.907 2396.152 56.592 139.347 163.940 198.888 392.141 637.350 1058.178 2336.510 4349.988 6481.772 7650.592 Cone, flag 390.48 bb 379.43 bb 381.75 bb 310.07 bb IDV *\ Y ) . )bnj w ' ffwjfwfvifyJs i6 12 O S I oi/ * 0.00 bb 2.98 bb 6.32 bb li:08 bb 36.01 bb 70.74 bb 128.01 bb 301.96 bb 575.94 MM 66.03 bbX 1025.08 bbX 14 0 30 27 15 9 4 4 -8 I* m ad a lin a 041099: :q u a n titn ta d an d p r in ta d b y m aa 5 /0 5 /9 9 000618 Q u an tify Conpound Sum uzy R apert Tex-130 R at L iv .r Sanpla U a t : H;\raU2.mo\SaiqplaDB\a4309Se Last audifiad: Thu Apr 2 2 09:03:11 1999 Mathod: H:\rata2.PRO\MathDB\042099o Laut modifiad: Tua Hay 04 09:53:4 1999 Jab Coda: Printad; Wad May OS 11:10:51 1999 BESTCOPYAVAIUBi! Paa 5 Compound 3s PFHfl Mama 1 042099002 2 042099003 3 042099004 4 042099005 5 042099006 6 042099007 7 042099008 8 042099009 9 042099010 10 042099011 11 042099012 12 042099013 13 042099014 14 042099015 15 042099016 16 042099017 17 042099018 18 042099019 19 042099020 20 042099021 21 042099022 22 042099023 23 042099024 24 042099025 25 042099026 26 042099027 27 042099028 28 042099029 29 042099030 30 042099031 31 042099032 32 042099033 33 042099034 34 042099035 35 042099036 36 042099037 37 042099038 38 042099039 39 042099040 40 042099041 41 042099042 42 042099043 43 042099044 44 042099045 45 042099046 46 042099047 47 042099048 48 042099049 49 042099050 50 042099051 51 042099052 52 042099053 S3 042099054 54 042099055 55 042099056 56 04209905757 042099058 58 042099059 59 042099060 <0 042099061 61 042099062 62 042099063 63 042099064 64 042099065 65 042099066 66 042099067 67 042099068 68 042099069 69 042099070 70 042099071 71 042099072 72 042099073 73 042099074 74 042099075 75 042099076 7 6 .04309907? 77 042099079 78 042099079 79 042099080 80 042099081 81 042099062 82 042099083 83 042099084 84 042099085 85 042099086 86 04209908? 67 042099088 88 042099089 Smplallit Taxt MaOH Blank TOX120, RSL04299-X2O81k-l, 4/19/99 TOX120, RBL04199-L1VBU-1, 4/19/99 TOX120, RBL04199-Sppb-1, 4/19/99 TOX120, RBL04199-10ppb-l, 4/19/99 TOX120, RBL04199-25ppb-1, 4/19/99 TOX120, RSL04199~50ppb-l, 4/19/99 TOX120, RBL04199-100ppb-l, 4/19/99 TOX120, RBL04199-250ppb-l, 4/19/99 T0X12, RBL04199-S00ppb-1, 4/19/99 Toxl'20, RBL04199-750ppb-l, 4/19/99 TOX120, RBL04199-1000ppb-l, 4/19/99 MaOH Blank ToxlZO, RTL, 1M, Gl, 4/19/99 TOX120, RTL, 2M, Gl, 4/19/99 TOX120, RTL, 3M, Gl, 4/19/99 TOX120, RTL, 4M, Gl, 4/19/99 Toxl20, RTL, 5M. Gl, 4/19/99 TOX120, RBL04199-2S0ppb-CCl, 4/19/99 MaOH Blank TOX120, RTL, CM# Gl, 4/19/99 Toxl20, RTL, 7M, Gl, 4/19/99 TOX120, RTL, 8M, Gl, 4/19/99 TOX120, RTL, 9M, Gl, 4/19/99 Toxl20, RTL, 10M, Gl, 4/19/99 Toxl20, RBL04199-250ppb-CC2, 4/19/99 MaOH Blank TOX120, RTL, 11M, Gl, 4/19/99 TOX120, RTL, 13M, Gl, 4/19/99 . TOX120, RTL, 14M, Gl, 4/19/99 TOX120, RTL, 1SH, Gl, 4/19/99 Toxl20, RBL04199-250ppb-CC3, 4/19/99 MaOH Blank TOX120, RTL, 17M, G2, 4/19/99 TOX120, RTL, IBM, G2, 4/19/99 Toxl20, RTL, 19M, G2, 4/19/99 TOX120, RTL, 2H, G2, 4/19/99 TOX120, RTL, 21M, G2, 4/19/99 TOX120, RBL04199-250ppb-CC4, 4/19/99 MaOH Blank TOX120, RTL, 22M, G2, 4/19/99 TX120, RTL, 23M, G2, 4/19/99 TOX120, RTL, 24M, G2, 4/19/99 TOX120, RTL, 25M, G2, 4/19/99 Toxl20, RTL, 26M, G2, 4/19/99 Toxl20, RBL04199-250ppb-CC5, 4/19/99 MaOH Blank ToxlZO, RTL, 27M, G2, 4/19/99 Toxl20, RTL, 29M, G2, 4/19/99 TOX120, RTL, 30M, G2, 4/19/99 TOX120, RTL, 31M, G2, 4/19/99 TOX120, RBL04199-25Oppb-CC6, 4/19/99 MaOH Blank TOX120, RTL, 33M, G3, 4/19/99 Toxl20,,RTL, 34M, G3, 4/19/99 TOX120, RTL, 35H, G3, 4/19/99 TOX12, RTL, 36H, G3, 4/19/99 Toxl20, RTL, 37M, G3, 4/19/99 TOX120, RBL04199-250ppb-CC7, 4/19/99 MaOH Blank TOX120, RTL, 38M, 63, 4/19/99 TOX120, RTL, 39M, G3, 4/19/99 TOX120, RTL, 40M, G3, 4/19/99 TOX120, RTL, 41H, G3, 4/19/99* Toxl20,* RTL, 42M, G3, 4/19/99 TOX120, RBL04199-250ppb-CC8, 4/19/99 MaOH Blank TOX120, RTL, 43M, G3, 4/19/99 Toxl20, RTL, 45M, G3, 4/19/99 . TOX120, RTL, 46M, G3, 4/19/99 TOX120, RTL, 47M, G3, 4/19/99 * TOX120, RBL04199-250ppb-CC9, 4/19/99 MaOH Blank TOX120, RTL, 65M, GS, 4/19/99 TOX120, RTL, 66M, GS, 4/X9/99 ToxlSO RTL, 73M, GS, 4/29/99 Toxl20, RTL, 7 4M 65* 4/19/99 TOX120, RTL, 7SM, 65, 4/19/99 Toxl20, RBL04l99-250ppb-CC4, 4/19/99 MOH Blank Toxl20, RTL, 77M G5, 4/19/99 TOX120, RTL, 78M, G5, 4/19/99 Toxl20, RTL, 79M, GS, 4/19/99 TOX120, RBL04199-2S0ppb-CCS, 4/19/99 * M0H Blank TOX120, RTL, 3M, 61-230ppb-MS, 4/19/99 Toxl20, RTL, 3M, Gl-250ppb-MSD, 4/19/99 Toxl20, RTL, 6M, Gl-250ppb-MS, 4/19/99 Typ Standard Standard Standard Standard Standard Standard Standard Standard Standard QC QC QC QC QC QC QC QC QC QC QC Btd Cono RT Aram Rasponaa Cono. Flaga %Oav 5.56 11.10 27.80 55*60 111.00 278.00 556.00 833.00 1111.00 4.160 4.158 4.154 4.112 4.156 4.118 4.117 4.114 4.117 278.00 4.162 4.155 4.161 4.154 4.118 4.116 278.00 278.00 4.161 4.159 4.115 4.160 4.158 4.112 4.160 4.162 4.118 4.159 4.118 99 179 502 895 1993 4901 10347 1516616551 99.365 179.476 502.222 895.168 1992.760 4900.550 ' 10347.100 15166.480 16551.121 1325 1876 965 . 995 607 5128 1324.885 1875.834 964.554 995.322 606.564 5127.719 966 792 823 854 * 4262 4828 965.683 792.578 823.111 853.907 4261.949 4828.117 2338 2072 1765 1326 5008 2337.712 2072.375 1764.636 1326.162 5008.266 4.87 HM 9.01 MM 25.67 MK 45.96 MM 102.63 MM 252.77 bb 534.00 bb 782.84 bb 854.34 MMX 68.15 KM 96.59 MM 49.54 MM 51.13 KM 31.06 MM 264.50 bb ' 49.60 bb 40.61 bb 42.24 MM 43.83 MM 219.80 bb 249.03 bb -12 -19 -8 -17 -8 -9 -4 -6 -23 \\\\- -10 120.44 bb 106.74 MM 90.8S bb 68.21 bb 258.33 bb -7 278.00 278.00 4.157 4.159 . 4.157 4.148 4.117 4.153 4.1SS 4.156 4.120 4.118 4.161 4.112 703 886 1144 2148 495 5496 562 ' 629 584 721 331 4659 702.749 885.923 1143.722 2147.549 494.722 5495.959 562.068 628.042 583.798 721.418 330.691 4658.773 36.02 MM 45.48 bb 58.79 bb 110.62 bb 25.28 bb 283.52 bb 28.76 bb 32.21 bb 29.86 bb 36.99 bb 16.81 MM 240.29 bb / / \c 2) I \\ -14 278.00 4.117 4.160 4.156 4.111 4.118 445 667 863 410 5427 * 445.452 666.912 862.746 . 409.525 5426.568 22.74 bb 34.17 bb 44.29 bb" 20.88 MM 279.93 bb . 1 278.00 4.158 4.157 4.113 4.131 4.133 4.130 1268 1021 1716 884 1278 4754* 1268.351 1021.077 1715.671 883.895 1278.325 4754.072 85.23 MM 52.46 MM 88.33 bb 45.38 bb 65.74 bb 245.21 MM -12 278.00 4.150 4.140 4.111 4.118 4.114 4.112 1086. 993 2036 445 646 5605 ' 1095.610 992.997 2036.141 445.27T 46.280 5605.275 55.79 MM 51.01 bb 104.87 bb ' 22.73 MM 33.11 MM 289.16 bb V/ / 278.00 278.00 278.00 4.116 4.112 4.114 4.117 .4.117 4.116 4.068 4.117 4.127 4.102 4.132 4.174 4*149 4.115 4.111 4.138 4.179 4.154 4.148 4.118 611 585 600 534 4623 . 1326573 1485431 569662 494912 582310 <459 245 331762 383053 302276 4714 115 6236 5869 6367 611.040 31.29 bb 585.165 29.95 MK 600.354 30.74 MM cVu4 P5D& A\533.884 27.30 bb - 4822.879 248.76 bb _ -11 1326572.750 1485431.125 68495.76 76698.23 bb bb J"' * i ... ... 29413.54 bbs 494911.688 25553.92 bb 582309.750 30066.62 bb p - e t A b X S b 6459.212 333.25 bb 245.376 12.41- MM 331762.219 17129.89 bb 383053.431 19778.25 bb 302275.969 15607.40 bb 4714.130 243.15 I -13 114.576 5. 65 MM 6236.417 321. 75 bb 5868.653 302. 76 bb ) E/tU tM 6366.802 328. 48 bb * / io g ) LAC os/os f a m a d a lin a 04 1 0 9 9 ; '.q u a n ti t a ta d an d p r i n t a d b y n a a 5 /0 5 /9 9 000619 O O o a K mad*lina 041099:-.quantitat*d a nd printad b y a m 3/05/99 Tox-120 Hat U w 22S2SSSSSS2SSSSS. 11 III I *E|U i !n ? H%* ***I* a t- ! 3 5'3C 5 I iis*rs s 2sa s S58 s s P 5 * " fc I 111" ? 3 SSSS I|& a| ESESSisas:. S8SS8SSSX 2 8 sSSSSssaSESSsSSes liiiis s ~ sssgl iiilig g g BggS BSSSSS3SSS333SSSI S 2 ! S 5 s 8 s . h MMS s 5 6 SSggSS2i2S:S2 ggSS3ggS3383ig&&3 . *H W A OH M* H MO D MH 8 i-J j < rSP Q u a n tify Compound B u m u ry R e p o rt Tox-120 R at L iv o r Sample Lit: N:\rata2.PR0Vsaopla0B\04209Sa Loot modified: Thu Apr 22 09:02: li 1999 Method: M:\rata2.PRO\MethD8\042099o Laat modified: Tue Hey 04 0S:S2:4S 1999 Job Code: Printed: Rad May OS 11:10:S1 1999 Compound 4: IS #Hama Sampialiat Text 1 042099002 MeOH Blank 2 042099003 Toxl20, RBL04199-H20Blk-l, 4/19/99 3 042099004 4 042099005 OX120, RBL04199-LivBlk-l, 4/19/99 Toxl20, RBL04199-5ppb-l, 4/19/99 6S 042099006 042099007 TOX120, RBL04199-10ppb-l, 4/19/99 Toxl20, RBL04199-2Sppb-l# 4/19/99 7 042099008 Toxl20. RBL04199-50ppb-l, 4/19/99 8 042099009 Toxl20, m04199-100ppb-l. 4/19/99 9 042099010 Toxl20, KBL04199-2S0ppb-l, 4/19/99 u10 042099011 042099012 Toxl20, RBL04199-500ppb-l, 4/19/99 Toxl20, ABL04199-?S0ppb-l, 4/19/99 12 042099013 Taxi20 RSL04199-1000ppb-l, 4/19/99 13 042099014 MeOH Blank 14 042099015 15 042099016 16 042099017 Toxl20, RTL, IK. SI. 4/19/99 Toxl20. RTL. 2M, SI. 4/19/99 Toxl20. RTL, 3M, Gl. 4/19/99 17 042099018 TOX120. RTL, 4M, 61, 4/19/99 18 042099019 Toxl20. RTL, SM, Gl, 4/19/99 1 042099020 Toxl20, RBL04199-2S0ppb-CCl, 4/19/99 20 042099021 MeOH Blank 21 042099022 TOX120, RTL, M. Gl, 4/19/99 22 042099023 TOX120. RTL, 7H. Gl, 4/19/99 23 042099024 Toxl20, RTL. BH. Gl, 4/19/99 24 042099025 TOX120, RTL, 9M, Gl, 4/19/99 25 042099026 26 042099027 TOX120, RTL, 10M, Gl, 4/19/99 TOX120, RBL04199-250ppb-CC2, 4/19/99 27 042099028 MeOH Blank 28 042099029 Toxl20, RTL. 11M, 6 1 , 4/19/99 29 042099030 Toxl2Q, RTL, 13M, Gl, 4/19/99 30 042099031 TOX120, RTL, 14M, Gl, 4/19/99 31 042099032 ` TOX120, RTL, ISM, Gl, 4/19/99 32 042099033 Toxl20, RBL04199-2S0ppb-CC3, 4/19/99 33 042099034 MaOH Blank 34 042099035 TOX120, RTL, 17M, G2, 4/19/99 35 042099036 TOX120, RTL, ISM, G2, 4/19/99 36 042099037 TOX120, RTL, 19M, G2, 4/19/99 37 042099038 TOX120, RTL. 20M, G2, 4/19/99 38 042099039 TOX120, RTL, 21M, G2, 4/19/99 39 042099040 TOX120, RBL04199-2S0ppb-CC4, 4/19/99 40 042099041 MeOH Blank 41 042099042 ' TOX120, RTL, 22M, G2, 4/19/99 42 042099043 Toxl20, RTL, 23M. 62, 4/19/99 43 042099044 TOX120, RTL, 24M, G2, 4/19/99 44 042099045 TOX120, RTL, 25M, G2, 4/19/99 45 042099046 TOX120, RTL, 26H, G2. 4/19/99 46 042099047 TOX120, RBL04199-2S0ppfa-CCS, 4/19/99 47 042099048 MaOH Blank 48 042099049 Toxl20, RTL. 27M, G2, 4/19/99 49 042099050 TOX120, RTL, 29M, G2, 4/19/99 50 042099051 Toxl20, RTL, 30M, G2, 4/19/99 51 042099052 TOX120, RTL, 31M. G2, 4/19/99 52 042099053 TOX120, RBL04199-2S0ppb-CC6, 4/19/99 53 042099054 54 042099055 MeOH Blank TOX120, RTL, 33M..G3, 4/19/99 55 042099056 56 042099057. 57 042099058 TOXI20, RTL, 34M, G3, 4/19/99 Toxl20, RTL, 35M, G3, 4/19/99 Toxl20, RTL, 3SM, G3, 4/19/99 58 042099059 Toxl20, RTL, 37M, G3, 4/19/99 59 042099060 ToxI20, RBL04199~2S0ppb-CC7, 4/19/99 60 042099061 MeOH Blank 61 042099062 TOX120, RTL. 36H, G3, 4/19/99 62 042099063 TOX120, RTL, 39M, G3, 4/19/99 63 042099064 TOX120, RTL, 4QM, G3, 4/19/99 64 042099065 TOX120, RTL, 41M, G3, 4/19/99 65 042099066 TOX12Q,* RTL, 42M, G3, 4/19/99 ' 66 042099067 TOX120, RBL04199-230ppb-CCS, 4/19/99 67 042099068 MeOH Blank 68 042099069 69 042099070 70 042099071 71 042099072 72 042099073 TOX120, RTL. 43H, G3, 4/19/99 TOX120, RTL, 4SM, G3, 4/19/99 TOX120, RTL, 44M, G3, 4/19/99 Toxl20, RTL, 47M, 63, 4/19/99 ' TOX120, RBL04199-2SOppb-CC9, 4/19/99 73 042099074 74 042099075 MeOH Blank TOX120, RTL, SSM, GS, 4/19/99 75 042099076 76 042099077 TOX120, RTL, (SK, GS, 4/19/99 TOX120, RTL, 73M, GS, 4/19/99 77 042099078 TOX120, RTL, 74M, G5, 4/19/99 78 042099079 TOX120, RTL, 7SH, GS, 4/19/99 79 042099080 TOX120, RBL04199-2S0ppb-CC4, 4/19/99 80 042099081 MeOH Blank 81 042099082 TOX120, RTL, 77M, GS, 4/19/99 82 042099083 Toxl2Q, RTL, 78M, GS, 4/19/99 83 042099084 Toxl20, RTL, 79M, GS, 4/19/99 84 042099085 TOX12Q, RBL04199-250ppb-CCS, 4/19/99 65 042099086 * 86 042099087 MeOH Blank TOX120, RTL, 3H, Gl-2S0ppb-M5, 4/19/99 87 042099098 TOX120, RTL, 3M, Gl-2S0ppb-MS0, 4/19/99 86 042099099 TOX120, RTL, 6M, Gl-2S0ppb-MS, 4/19/99 TVpe S td C otta Standard Standard Standard Standard Standard Standard Standard Standard , Standard 1.00 1 a00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 QC 1.00 OC . QC 1.00 1.00 QC 1.00 QC 1.00 QC 1.00 QC 1.00 QC 1.00 QC 1.00 QC 1.00 . QC 1.00 xr 4.67 4.477 4.477 4.475 4.472 4.474 4.473 4.481 4.4-78 4.475 4.47 4.477 4.473 4.479 4.473 4.480 4.477 4.479 4.476 4.478 4.478 4.476 4.475 4.476 4.479 4.479 4.476 4.479 4.474 4.476 4.475 4.465 4.434 4.471 4.473 4.474 4.438 4.434 4.434 4.473 4.478 4.434 4.473 4.429 4.478 4.475 4.474 4.430 4.445 4.448 4.445 4.467 4.456 4.426 4.437 4.475 4.475 4.434 4.474 4.475 4.435 4.478 4.478 4.475 4.434 4.442 4.461 4.449 .4.465 4.473 4.428 4.453 4.472 4.466 4.480 A to m 11168 14262 17108 14220 14163 15047 14165 12687 13127 12184 14980 13354 15480 16743 16108 16428 12965 12592 12908 14767 13113 . 16767 15329 . 14482 11815 13252 12072 12820 7188 6839 6975 7305 7576 15008 7420 8272 8265 9236 9268 14716 8715 12268 10776 11197 14400 16537 8276 7717 9574 7747 15240 7589 9947s 7538 8461 12183 .14952 8922 9854 13112 9645 15910 10254 11430 14854 14617 14512 15752 26825 16234 16282 15674 15718 17154 15585 tOvX l t p O R M C o tta flag * 11168.010 14262.124 17107.816 14220.119 14162.521 15047.055 14164.800 12686.997 13127.305 12183.721 14980.457 0.72 bb 0.92 bb 1.10 bb 0.92 bb 0.91 bb 0.97 bb 0.91 bb 0.82 bb 0.85 bb 0.79 bb 0.97 M M -28 -8 10 -8 -9 -3 -9 -19 -15 -21 -3 13353.618 15479.964 16743.496 16107.631 16427.918 12964.758 0.96 bb 1.00 bb 1.09 bb 1.04 bb 1.06 bb 0.84 bb -14 0 8 4 6 -16 12591.617 12908.252 14767.411 13113.133 16766.613 15328.990 0.81 bb 0.83 bb 0.95 bb . 0.85 bb 1.08 bb 0.99 bb -19 -17 -5 -158 -1 14482.320 11815.149 13252.295 12071.706 12819.677 0.93 bb 0.76 bb 0.86 bb 0.78 bb 0.83 bb -7 -24 -14 -22 -17 7188.418 6839.444 6975.442 7304.985 7576.105 15007.997 0.46 bb 0.44 bb 0.45 bb 0.47 bb 0.49 bb 0.97 bb -54 -56 -55 -53 -51 -3 7419.602 8272.232 8264.774 9235.608 268.021 14716.280 0.48 bb 0.53 bb 0.53 bb 0.60 MM 0.60 bb 0.95 bb -52 -47 -47 -40 -40 -5 8714.930 12268.174 10776.486 11196.844 14399.545 0.56 bb 0.79 bb 0.70 bb, 0.72 bb 0.93 bb , -44 -21 -30 -28 -7 16537.041 8276.272 7716.823 9574.318 7747.233 15240.495 1.07 bb 0.53 bb 0.50 bb 0.62 bb 0.50 bb 0.98 bb 7 -47 -50 -38 -50 -2 7588.534 9947.499 7537.861 480.613 12182.729 14951.941 0.4 bb 0.64 bb 0.49 bb 0.55 bb 0.79 bb 0.97 bb -51 -36 -51 -45 -21 -3 8921.938 9854.359 13111.587 . 9645.204 15909.816 0.58 MM 0.64 bb 0.85 bb 0.62 bb 1.03 bb -42 -36 -15 -38 3 10253.570 11430.374 14853.702 14617.353 14511.814 15752.205 0.66 bb 0.74 bb 0.96 MM 0.94 bb 0.94 bb 1.02 bb -34 -26 -4 -6 -6 2 26824.648 16234.444 16281.634 15674.262 1.73 bb 1.05 MM 1.05 MM 1.01 bb 73 5 S 1 15717.900 17154.322 15585.048 1.01 bb 1.11 bb 1.01 bb 1 11 1 Pape 7 M ad elin e 0 4 1 0 9 9 :q u a n tita te d and p r in te d b y m aa 5 /0 S /9 9 000621 Q u a n tif y Com pound Summary R a p o rt Tox-120 S a t L iv a r Sample Liat: H:\rata2.PSO\SaapleDB\Q42099e Laat modified: Thu Apr 22 09:02:11 1999 Mathod: N :\rata2. VS0\MethD8\O42O99o Laat modified: Tua Hay 04 09:52:49 1999 Job Coda: Printed: Wad Hay 05 11:10:51 1999 Compound 4: 15 Mama 99 042099090 90 042099091 91 042099092 92 042099093 93 042099094 94 042099095 95 042099096 95 042099097 97 042099098 98 042099099 99 042099100 100 042099101 101 042099102 102 042099103 103 042099104 104 042099105 Saapl*liat Taxt Typ* Std'Cono TOX120, RTL, CM, Gl-250ppb-MSD, 4/19/99 TOX120, RTL, 13M, Gl-2S0ppb-MS, 4/19/99 TOX120, RTL, 13H, 61-2S0ppb-M5D, 4/19/99 OX120, RBL04199-2iOppb-CC, 4/19/99 QC 1.00 HaOH Blank TOX120, RBL04199-H2OBlk-l, 4/19/99 TOX120. RBL04199-LivBlk-l, 4/19/99 TOX120, RBL04199-- 5ppb~l, 4/19/99 TOX120, RBL04199-10ppb-l, 4/19/99 TOX120, RBL04199-25ppb-l, 4/19/99 TOX120, RBL04199-S0ppb-1, 4/19/99 TOX120, RBL04199-100ppb-l, 4/19/99 TOX120, RBL04199-2S0ppb-l, 4/19/99 TOX120, RBL04199-S00ppb>l, 4/19/99 TOX120, RBL04199-7SOppb-l, 4/19/99 Toxl20, RBL04199-1000ppb-l,-4/19/99 Standard Standard Standard Standard . Standard Standard Standard Standard Standard 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 M 4.477 4.478 4.435 4.470 4.478 4.478 4.473 4.435 4.433 4.434 4.433 4.465 4.434 4.434 4.435 Pago 8 Araa 15039 14583 15562 16369 13605 17110 20728 17142 16514 17079 17088 15845 15402 15262 16108 Response 15038.934 14562.552 15562.266 16367.936 13604.745 17109.813 20728.434 17141.998 16513.951 17078.793 17087.787 15644.741 15402.126 15261.598 16108.356 Cone. Flaoa %Dav 0.97 bb -3 0.94 bb -6 1.00 bb 0 1.06 bb 6 0.68 bb 1.10 bb 1.34 bb 1.11 bb 1.07 bb 1.10 bb 1.10 bb 1.02 bb 0.99 bb 0.99 MM 1.04 bb -12 10 34 11 7 10 10 2 -1 -1 4 .!>t m ad elin e 0 4 1 0 9 9 ::q u a n tita ta d and p r in ta d b y aa a 5 /0 5 /9 9 000622 Q u a n tify C a lib ra tio n fiap o rt T ox-120 H at L iv a r Calibration s W:\rata2.PH0\CurvaDB\042099o Last tnodifiad: W o d M ay 05 09:00:19 1999 Printad: Wad May 05 11:11:10 1999 ^Compound 1 name: POAA Coefficient o f Detennination: 0.989036 1 m ad alin a 0 4 1 0 9 9 :tq u a n tita ta d and p r in ta d b y n aa 5 /0 5 /9 9 000623 Q u an tify C a lib ra tio n R aport Tox-120 R a t L iv a r Calibration: M:\rata2.FRO\Curva0B\042099a Laat nodifiad: Had May OS 09:00:19 1999 Frintad: Rad May OS 11:11:10 1999 Vago 2 m ad a lin a 041099: :q u a n ti ta ta d and p r in ta d b y m an 5 /0 5 /9 9 000624 Q u in tiy C a lib ra tlo n R aport Tox-120 R at L iv a r Calibration: M:\rata2.VRO\CurvaDB\042099e List nodifiad: Rad May 03 09:00:19 1999 Printad: Rad Kay OS 11:11:10 1999 Vaga 3 n id a lin a 041099: : q u a n ti ta t a d an d p r in ta d b y M a S/O S/99 000625 Quantify Calibration Kaport Tea-120 tat Llvar Calibration: M:\rats2.mo\CurvaDB\042099a Last nodifiad: Wad May OS 09:00:19 1999 Prlntad: Wad May OS 11:11:10 1999 ' Pag 4 a a d a lin a 041099: iq u a n tita ta d and. p r in ta d b y n aa S /0 S /9 9 000626 H.thod Report Method t i l t : Last modiil.d: Compound: Printed: N:\raCs2.PRO\HethOB\042099c.mdb Tu Hey 04 0S:S2:4S 1999C 1: POAA Had Hey OS 11:10:2 1999 Compound N am: Internal Ref.: Qutnify Traa: Conc. of Standards: POAA (Nona) TIC Cone. A Usar RF Vala: Usar Psak Factor: Integrate Window Factor: 1.000000, Dlsablad 1.000000 2.000 Peak Location Ratantion Tima (mine): Relative Ratantion Tina: Tina Window (nina): 4.400, Enabled 0.000, Disabled 0.834 Faak Salactlon: Nearest Rasoonaa ] Raaponsa Typa: Rasponsa: Calibration Curves External Areas Polynomial Typa: 1 Point of Origin: Fit Weighting: Axis Transformation: . Linear Exclude 1/X Nona Concentration ] Units: Noise Peak-to-'peak amplitude 434 Smooth Smoothing: Window sisa (scans): Numbar of smooths: Smoothing method: Disabled 3 2 Baselines Join valley threshold: Reduce peak tailing: Raisa basaliaa maximum: 20.00 30.00 5.00 Peak Senaration Draw vertical threshold: Detect shoulders: Shoulder threshold: : 10.00 Disabled 40.00 J Response Threshold Relativ height: Absolute height: Relative area: Absolute area: 1.50, Disabled 0.00, Disabled ' 2.00, Disabled 0.00, Disabled 3 ] I l'*0. 1 I LAC/ oslof h ? t* * t `f i f 000627 r * ! K.tfiod Report Method file: Last modified: Compound: Printed: N : \ r t j 2 .P R O \ M * t h O B \ 0 4 2 0 9 9 c . a d b Tu. May 04 04:52:4* 19990 2: Pros Had Hay 05 11:10:26 1999 Compound Name: Internal Ref.: Quantity Trace: Cone*, of Standards pros (Hone] TIC Cone. A User ftp Value: User Peak Factor: Integrate Window Factor; 1.000000, Disabled 1.000000 2.000 Peek Location Retention Time Ulna): Relative Retention Tine: Time Window (mins): 4.790, Enabled 0.000, Disabled 0.034 Peak Selection: Nearest Response Response Type: Response: Estensi Areas Calibration Curves Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Linear Exclude 1/X None Concentration Units: Noise Paak-to-peak amplitude: 434 Smooth Smoothing; Window size (scans) Number of smooths: Smoothing method: Disabled 3 2 Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: 20.00 50.00 a. 5.00 Peak Seoaration Draw vertical threshold: Detect shoulderj; Shoulder threshold: . 10.00 Disabled 40.00 Reseonse Threshold Relative height: Absolute height: Relative area: Absolute area: 1.50, Olaablad 0.00, Disabled * 2.00, Diaablad 0.00, Disabled Rage 2 M fljtlihi, Wl(M lAC. n ila tk _ _ _ _ _ _ _ A*4 000628 Method Report Method file: Lest modified: Compound: Printed: N:\rats2.PRO\MethDB\042099c.mdb Tue May 04 00:52:48 19990 3: PFHS Med May 05 11:10:26 1999 Compound Name: Internal Ref.: Quantify Trace: Cone', of Standards: User RF Value: User Peak Factor: Integrate Window Factor: Peak Location Retention Time (mins): Relative Retention Time: Time Window (mins]: Peak Selection: Response Response Type: Response: Calibration Curves Polynomial Type: Point o Origin: Fit Weighting: Axis Transformation: Concentration Units: Noise Peak-to-peak amplitude: Smooth Smoothing: Window size (scans): Number of smooths: Smooching method: Basellnes 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 aree: Absolute area) PFHS (None) TIC Cone. A 1.000000, Disabled 1.000000 2.000 4.120, Enabled 0.000, Disabled 0.834 Nearest External Areas Linear Exclude 1/X None 434 Disabled 3 2 20.00 50.00 5.00 10.00 Disabled 40.00 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled H & cI lL , OHIdW LAC/ o r / c ^ M 3 .X 000629 Mechad Report Method file: Last Modified: Compound: Printed: N:\r.t32.PR0\M.thDB\042099e.mdb Tue May 04 08:52:49 1999Q 4: IS Ned M ay OS 11:10:26 1999 Compound Name: Internal Ref.: Quantify Trace: ConC of Standard: , IS (None) TIC Fixed User RF Value: User Peak Factor: Integrate Window Factor: 1.000000* Disabled 1.000000 2.000 Peak Location Retention Time (mins): Relative Retention Time: Time Window (mins): 4.480, Enabled 0.000, Disabled 0.834 Peak Selection: N.r.it Resoonse Response Type: Response: External Areas Calibration Curves Polynomial Type: Point of Origin: Tit Weighting: Axis Transformation: Linear Exclude 1/X None Concentration Unita: Noise Peak-to-peak amplitude: 434 Smooth Smoothing: Window sire (scans): Number of smooths: Smoothing method: Disabled 3 2 Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: 20.00 50.00 5.00 Peak Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: t 10.00 Disabled 40.00 Response Threshold Relative height: Absolute height: Relative area: Absolute area: 1.S0, Disabled 0.00, Disabled 4 2.00, Disabled 0.00, Disabled M a A tU c h ip Pag* 4 000630 AM ELIA062498: FACT Equipm ent Log 99016 Q uattro H , #6448E PAGE DATE: 04/20/99 ANALYST: mee STUDY NUMBER Tox-120 MATRIX: R at Liver DESCRIPTION: ip FACT M ethod: ETS-8-5.0________ Injection volume,10 uL Cycle tim e: 9.0 m in. Electrode: Z-Spray M obile P hase: (A12.0 mM NH4GH3CQ2 (B)M eO H TN-A- or stndrd num ber (A ) 99012-5-22_________ (B) TN-A-2414 Prepared (date/by): (A) 4/16/99 / ok_________ (B) 4/9/99 hoj E x p ires: (A) 10/99_______________ (B) 10/99 Store at room temp? |Y| o r N O ther:___________________ G u ard colum n: N one ______________ P art num ber na_________ Lot number: na______________________ A nalytical colum n: keystone betasil ___________________________________ Size: 2 x 50mm_________________ Type: c l8____________ Sphere size: 5 um Part number: 055-701-2 L ot num ber P7L04 Serial num ber 0481172z A nalytical param eters: t D rying gas (L/hr): 300 ESI nebulizing gas (L/hr) 15 LC Flow rate: 300 ulVmin. Back pressure: 59 bar Sheath gas (L/hr)_0___ H PLC solvent g rad ien t: long2 Time (m in.) 1) 0.00________ 2) 4.5__________ . 3 6.5_________ 5) 7.0_________ 6) 9.0__________ %B 40 95 95 40 stop 000631 Tuning Method Report Method: C:\MASSLYNX\RATS2.PRO\ACQUDB\PFOS Printed: Tue Apr 20 17:06:38 1999 ' Page 1 SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. Set Rdbk 3.00 15 5 0.2 150 250 2.99 -14 -6 152 258 Pressures Analyser Vacuum Cas Cell Rdbk 1.6e-4 4.7e-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier Set Rdbk 15.0 15.0 2.0 s o.o- 57 650 MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set Rd 15.0 15.0 30 2.0 0.0 40 0 650 32 39 30 000632 FACT: DATA REVIEW SUMMARY FORM Date: 4 /^ /5 2 Analyst: H FACT Studv Number W ' M Matrix ILf Tuna Pointa M f 4 Dilutions? YJLtdJ- Analyte 1: AcccotableT,mftarRange: LOQ for Aia data set _______ ^ Reevaluated for differentrange? M Analyte 4: Acceptable Linear Range: / LOQ for this data set / Re-evaluated for differentrange? / / ____________________ _____ for different range? Analvte2: ./ Acceptable Linear Range: LOQ for this data set .f Re-evaluated for different range? - J . ____________ Analyte 3:. Acceptable Linear Range: LOQ for this data set: Re-evaluated far different Analyte 6: Acceptable linear Range: LOQ for diis data set Re-evaluated for differentrange? Analyte 7: Acceptable Linear Range: LOQ for this data set Re-evaluated for different range? h ilL j ly v d r C fiv J e l b * k u /b * ~ ' 000633 Q u a n tif y Com pound flutto*r y l u p o r t Saaplo Lit: C:\MA8SLYKX\rata2. FR0\SaoplaDB\042099d Last aodifiad: Thu Apr 22 07:25:34 1999 Mathod: C:\HA38LYHX\rmta2. PRO\MothDB\042099d Last oodifiad: Thu Apr 22 07:23:52 1999 Job Coda: Printod: Thu Apr 22 07:31:55 1999 Compound 1$ " I iiaaa 1 04209910 2 042099107 3 042099100 4 042099109 5 042099110 0 042099111 7 042099112 8 042099113 9 042099114 10 042099115 11 042099116 12 042099117 13 042099110 14 042099119 15 042099120 16 042099121 17 042099122 U 042099123 19 042099124 20 042099125 21 042099126 22 042099127 23 042099128 24 042099129 25 042099130 26 042099131 27 042099132 28 042099133 29 042099134 30 042099135 31 042099136 32 042099137 33 042099138 34 042099139 35 042099140 36 042099141 37 042099142 38 042099143 39 042099144 40 042099145 41 042099146 42 042099147 43 042099148 44 042099149 Saxploliat Taxt MtOH BlftJe 10x120, RBL04199-H20Blk-l, 4/19/99 Toxl20, RBL04199-LivBlk-l, 4/19/99 TOX120, RBX04199-5ppb-l, 4/19/99 TOX120, RBL04199-10ppb-l, 4/19/99 TOX120, ABL04199-2Sppb-l, 4/19/99 TOX120, RBt04199-50ppb-l, 4/19/99 Toxl20, RBL04199-100ppb-l, 4/19/99 Toxl20, RB104199-250ppb-l, 4/19/99 TOX120, RBL04199-S00ppb-1, 4/19/99 TOX120, RBL04199-750ppb-l, 4/19/99 TOX12Q, RBL04199-1000ppb-l, 4/19/99 KaOH Blank TOX120, ATI, 49H, 64, 4/19/99 TOX120, RTL, 50M, 64, 4/19/99 Toxl20, RTL, 51M, 64, 4/19/99 TOX120, RT1, S2M, 64, 4/19/99. TOX120, RTL, 53M, 64, 4/19/99 TOX120, RBL04199-2$0ppb-CCl, 4/19/99 MaOK Blank Toxl20, RTL, 54M, 64, 4/19/99 Toxl20, RTL, 55H, 64, 4/19/99 TOX120, RTL, 56M, 64, 4/19/99 TOX120, RTL, 57M, 64, 4/19/99 oxl20, RTL, S8H, G4, 4/19/99 TOX120, RBL04199-250ppb-CC2, 4/19/99 HaOH Blank TOX120, RTL, S9M, G4, 4/19/99 Toxl20, RTL, 61M, 64, 4/19/99 Toxl20, RTL, 62M, 64, 4/19/99 TOX120, RTt, 63M, G4, 4/19/99 TOX120, RBL04199-250ppb-CC3, 4/19/99 KeOK Blank Toxl20, RBU)4l99-H20Blk-l, 4/19/99 TOX120, RBU>4l99-LivBlk-l, 4/19/99 TOX120, RBL04l99-5ppb-l, 4/19/99 TOX120, RBL04199*1Oppb-1, 4/19/99 TOX120, RB104199-25ppb-l, 4/19/99 TOX120, RBl04l99-50ppb-l, 4/19/99 Toxl20, RB104199-I00ppb-1, 4/19/99 TOX120, RB104199-250ppb-l, 4/19/99 Toxl20, RBI*04199-S00ppb-1, 4/19/99 Toxl20, RBI*04199-7S0ppb-l, 4/19/99 TOX120, RBL04199-1000ppb-l, 4/19/99 Pag 1 Typa Standard Standard Standard Standard Standard Standard Standard Standard Standard QC OC QC Standard Standard Standard Standard Standard Standard Standard Standard Standard fltd Ceno 5.00 10.00 25.00 50.00 100.00 250.00 500.00 750.00 1000.00 250.00 250.00 250.00 5.00 10.00 25.00 50.00 100.00 250.00 500.00 750.00 1000.00 RT 4.631 4.574 4.770 4.766 4.770 4.768 4.746 4.743 4.746 4.743 4.743 4.745 4.436 4.728 4.746 4.754 4.745 4.747 4.731 4.502 4.746 4.724 4.747 4.791 4.764 4.742 . 4.502 4.766 4.756 , 4.770 4.762 4.747 4.418 4.528 4.768 4.766 4.764 4.763 4.765 4.766 4.763 4.768 4.750 4.755 A m Cono. Plaga %Dav 12 0.00 b b 40 0.95 bb 36 0.00 bb 57 5.24 bb 5 89 13.82 MM 39 155 31.66 MM 27 247 56.22 bb 12 485 120.05 bb 20 * 1112 287.94 MM 15 2185 575.32 bb IS 2976 787.41 bb 5 3297 873.36 bbX -13 87 13.52 bb 12991 3470.15 bb 6082 1619.43 bb 5703 1517.85 bb I 7024 1871.64 bb 2063 543.96 bb 1057 273.37 bb 9 100 16.96 MM 6163 1641.02 bb rv 9346 2627*60 bb 11879 3172.37 bb 651 164.53 bb 150 30.42 bb 1017 262.59 bb * 5 124 23.19 bb 772 196.94 bb 155 31.70 bb 189 40.35 bb 60 6.26 bb 977 251.92 MM 1 107 18.64 bb 26 0.00 bb 33 0.00 bb 51 3.82 bb -24 S3 4.34 bb -57 111 19.80 bb -21 225 50.35 MM 1 397 96.32 MM -4 864 221.52 bb -11 1745 457.44 bb -9 2459 648.75 bb -13 2343 7S1.70 MMX -25 p. Amalia 062493: Raviavad and quanti tatad by kjh 4/22/99 000634 Q u an tity C a lib ra tio n a n p o rt Calibrations C:\MASSUmx\rata2.91IO\CurvaDB\042099d Laat noditlad: Thu Apr 22 07:30:53 1*9 Printed: Thu Apr 22 07:31:55 19*9 Pago 1 Anal la 052495: Aavlawad and quantitated by k)h 4/22/9 000635 Masslynx - Sample List Sample Ust: C:\MASSLYNX\rats2.PRO\SampleDB\042099c.SPL Printed: Tue Apr 20 16:51:50 1999 F ile Nam e F ile T ext 1 042099002 MeOH Blank 2 042099003 Tox120, R B L04199-H 2O B Ik-t, 4/19/99 3 042099004 Tox120, RBL04199-LivBlk-1,4 /1 9 /9 9 4 042099005 Tox120, R B L04199-5ppb-1,4/19/99 5 042099006 Tox120, R B L04199-10ppb-1,4/19/99 6 042099007 Tox120, RBL04199-25ppb-1,4 /1 9 /9 9 7 042099008 Tox120, R B L04199-50ppb-1.4/1 9 /9 9 8 042099009 Tox120, RBL04199-100ppb*1,4 /1 9 /9 9 9 042099010 Tox120, RBL04199-250ppb-1,4 /1 9 /9 9 10 042099011 TOX120, R BL04199-500ppb-1,4 /1 9 /9 9 11 042099012 Tox120, RBL04199-750ppb-1,4 /1 9 /9 9 12 042099013 Tox120, RBL04199-1000ppb-1,4 /1 9 /9 9 13 042099014 MeOH Blank 14 042099015 Tox120, RTL, 1M , G 1 ,4/1 9 /9 9 15 042099016 Tox120, RTL. 2M , G 1 ,4/1 9 /9 9 16 042099017 Tox120, RTL. 3M . G 1 .4/1 9 /9 9 17 042099018 Tox120, RTL. 4M . G 1 .4/19/99 18 042099019 Tox120, RTL. 5M , G 1 ,4/1 9 /9 9 19 042099020 Tox120, R B L04199-250ppb-C C 1,4/1 9 /9 9 20 042099021 MeOH Blank 21 042099022 Tox120, RTL, 6M . G 1 ,4/19/99 22 042099023 Tox120, RTL, 7M , G 1 .4/19/99 23 042099024 Tox120, RTL, 8M , G 1 ,4/19/99 24 042099025 Tox120, RTL, 9M , G 1 ,4/19/99 25 042099026 Tox120, RTL. 10M , G 1 ,4/19/99 26 042099027 Tox120, R B L04199-250ppb-C C 2,4/19/99 27 042099028 MeOH Blank 28 042099029 Tox120, RTL, 11M , G 1 ,4/19/99 29 042099030 Tox120, RTL, 13M , G 1 ,4/19/99 30 042099031 Tox120, RTL, 14M , G 1,4 /1 9 /9 9 31 042099032 Tox120, RTL, 15M , G 1,4 /1 9 /9 9 32 042099033 Tox120, R B L04199-250ppb-C C 3,4/19/99 33 042099034 MeOH Blank 34 042099035 Tox120, RTL, 17M , G 2 ,4/19/99 35 042099036 Tox120, RTL. 18M , G 2 ,4/19/99 36 042099037 Tox120, RTL, 19M , G 2 ,4/19/99 37 042099038 Tox120, RTL, 20M , G 2 ,4/19/99 38 042099039 Tox120, RTL, 21M , G 2 ,4/19/99 39 042099040 Tox120, R B L04199-250ppb-C C 4,4/19/99 40 042099041 M eO H Blank 41 042099042 Tox120, RTL. 22M , G 2 ,4/19/99 42 042099043 Tox120, RTL, 23M , G 2 ,4/19/99 43 042099044 TOX120, RTL, 24M , G 2 .4/19/99 44 042099045 T o x t2 0 , RTL, 25M , G 2 .4/19/99 45 042099046 Tox120, RTL, 26M , G 2 ,4/19/99 46 042099047 Tox120, R B L04199-250ppb-C C 5,4/19/99 47 042099048 M eO H Blank 48 042099049 Tox120, RTL, 27M , G 2 ,4/19/99 49 042099050 Tox120, RTL, 29M , G 2 ,4/19/99 50 042099051 Tox120, RTL, 30M , G 2 ,4/19/99 51 042099052 Tox120, RTL, 31M , G 2 ,4/1 9 /9 9 52 042099053 Tox120, R B L04199-250ppb-C C 6,4/19/99 53 042099054 MeOH Blank 54 042099055 TOX120, RTL, 33M , G 3 ,4/1 9 /9 9 55 042099056 Tox120, RTL, 34M , G 3 ,4/19/99 56 042099057 Tox120, RTL, 35M , G 3 ,4/1 9 /9 9 57 042099058 Tox120, RTL, 36M , G 3 ,4/19/99 58 042099059 Tox120, RTL, 37M , G 3 ,4/19/99 59 042099060 Tox120, R B L04199-250ppb-C C 7,4/19/99 60 042099061 MeOH Blank y /^ y y 7 Page 1 MS File In let File 9MIN-COMBI7IS-POAA 9mln 9M IN-COMBI7IS-POAA 9min 9M IN-COMBI7IS-POAA 9min 9M IN-COMBI7IS-POAA 9mln 9M IN-COMBI7IS-POAA 9min 9MIN-COMBI71S-POAA 9min 9M IN-COMBI7IS-POAA 9mln 9MIN-COMBI7IS-POAA 9min 9MIN-COMBI7IS-POAA 9min 9M IN-COMBI7IS-POAA 9mln 9MIN-COMBI71S-POAA 9min 9M IN-COMBI7IS-POAA 9mln 9M IN-COMBI7IS-POAA 9mln 9M1N-COMBI7IS-POAA 9min 9M IN-COMBI7IS-POAA 9min 9M IN-COMBI7IS-POAA 9min 9MIN-COMBI7IS-POAA 9min . 9MIN-COMBI7IS-POAA 9min 9M IN-COMBI7IS-POAA 9min . 9MIN-COMBI7IS-POAA 9mln 9MIN-COMBI7IS-POAA 9min 9M IN-COMBI7IS-POAA 9min 9MIN-COMBI7IS-POAA 9mln 9MIN-COMBI7IS-POAA 9min 9M IN-COMBI7IS-POAA 9niln 9M IN-COMBI7IS-POAA 9min 9MIN-COMB17IS-POAA 9min 9M IN-COMBI7IS-POAA 9mln 9MIN-COMB17IS-POAA 9min 9MIN-COMBI7IS-POAA 9mln 9MIN-COMBI7IS-POAA 9min 9M IN-COMBI7IS-POAA 9min 9M IN-COMBI7IS-POAA 9min 9M IN-COMBI7IS-POAA 9min 9M IN-COMBI7IS-POAA - 9min 9MIN-COMBI7IS-POAA 9mln 9MIN-COMBI7IS-POAA 9mln 9M IN-CO M BI7IS-PO A A . 9mln 9M IN-COMBI7IS-POAA . 9min 9MIN-COMBI7IS-POAA 9mln 9MIN-COMBI7IS-POAA 9min 9MIN-COMBI7IS-POAA 9min 9MIN-COMBI7IS-POAA 9mln 9M IN-COMBI7IS-POAA 9mln 9M IN-COMBI7IS-POAA 9mln 9M IN-COMBI7IS-POAA 9min 9M IN-COMB17IS-POAA 9 M IN -C O M B 17IS -P O A A 9M IN-COMBI7IS-POAA 9min 9mln 9mln 9M IN-COMBI7IS-POAA 9min 9M IN-COMBI7IS-POAA 9mln 9M IN-COMBI7IS-POAA 9mln 9M1N-COMBI7IS-POAA 9min 9M IN-COMBI7IS-POAA 9min 9M IN-COMBI7IS-POAA 9min 9MIN-COMBI7IS-POAA 9min 9MIN-COMBI7IS-POAA 9min 9M IN-COM B17IS-POAA 9min 9M IN-COMBI7IS-POAA 9min 9M IN-COMBI7IS-POAA 9mln B o ttle 91 1 2 3 4 5 6 7 8 9 10 11 * 91 12 13 14 15 16 81 92 17 18 19 20 21 82 92 22 23 24 25 83 92 26 27 28 29 30 84 92 31 32 33 34 35 85 92 36 37 38 39 86 93 40 41 42 43 44 87 93 000636 Masslynx - Sample List Sample List: C:\MASSLYNX\rats2.PRO\SampleDB\042099c.SPL Printed: Tue Apr 2016:51:50 1999 F ile Nam e 61 042099062 62 042099063 63 042099064 64 042099065 65 042099066 66 042099067 67 042099068 68 042099069 69 042099070 70 042099071 71 042099072 72 042099073 73 042099074 74 042099075 75 042099076 76 042099077 77 042099078 78 042099079 79 042099080 80 042099081 81 042Q99082 82 042099083 83 042099084 84 042099085 85 042099086 86 042099087 87 042099088 88 042099089 89 042099090 90 042099091 91 042099092 92 042099093 93 042099094 94 042099095 95 042099096 96 042099097 97 042099098 98 042099099 99 042099100 100 042099101 101 042099102 102 042099103 103 042099104 104 042099105 F ile T ext Tox120, RTL, 38M , G 3 ,4/19/99 Tox120, RTL, 39M , G 3 .4/19/99 TOX120, RTL, 40M , G 3 ,4/19/99 Tox120, RTL, 4 1 M , G 3 ,4/19/99 Tox120, RTL, 42M , G 3 ,4/19/99 Tox120, R B L04199-250ppb-C C 8,4/19/99 MeOH Blank TOX120, RTL, 43M , G 3 ,4/19/99 TOX120, RTL, 45M , G 3 ,4/19/99 Tox120, RTL, 46M , G 3 ,4/19/99 Tox120, RTL, 47M , G 3 ,4/19/99 Tox120, R B L04199-250ppb-C C 9,4/19/99 MeOH Blank TOX120, RTL, 65M , G 5 ,4/19/99 Tox120, RTL, 66M , G 5 ,4/19/99 Tox120, RTL, 73M , G 5 ,4/19/99 TOX120, RTL, 74M , G 5 ,4/19/99 TOX120, RTL, 75M , G 5 ,4/19/99 Tox120, R B L04199-250ppb-C C 4,4/19/99 MeOH Blank Tox120, RTL, 77M , G 5 ,4/19/99 Tox120, RTL, 78M , G 5 ,4/19/99 Tox120, RTL, 79M , G 5 ,4/19/99 TOX120, RBL04199-250ppb-CC5, 4/19/99 M eO H Blank Tox120, RTL, 3M , G1-250ppb-M S, 4/19/99 TOX120, RTL, 3M . G1-250ppb-M SD, 4/19/99 TOX120, RTL, 6M , G1-250ppt>-MS, 4/19/99 Tox120, RTL, 6M , G 1-250ppb-M SD, 4/19/99 Tox120, RTL, 13M , G1-250ppb-M S, 4/19/99 Tox120, RTL, 13M , G1-250ppb-M SD, 4/19/99 Tox120, R BL04199-250ppb-C C 6,4/19/99 M eO H Blank Tox120, R B L04199-H 2O B Ik-1,4/19/99 Tox120, RBL04199-LivBlk-1,4 /1 9 /9 9 TOX120, RBL04199-5ppb-1,4 /1 9 /9 9 TOX120, RBL04199-1 Oppb-1,4 /1 9 /9 9 TOX120, R B L04199-25ppb-1,4/19/99 Tox120, RBL04199-50ppb-1,4 /1 9 /9 9 Tox120, RBL04199-100ppb-1,4/19/99 TOX120, RBL04199-250ppb-1,4 /1 9 /9 9 Tox120, R BL04199-500ppb-1,4/19/99 TOX120, RBL04199-750ppb-1,4 /1 9 /9 9 TOX120, RBL04199-1000ppb-1,4 /1 9 /9 9 Page 2 MS File 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M N-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M INrCOM BI7IS-POAA . 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M 1N -C O M B I7IS -P O A A 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN -C O M B I71S -P O A A 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M 1N -C O M B I7IS -P O A A 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA 9M IN-CO M BI7IS-POAA In let F ile 9min 9min 9min 9min 9mln 9min 9min 9min 9min 9mln 9min 9min 9min 9min 9mln 9mln 9min 9min 9mJn 9m in. 9min 9min 9min 9min 9mln 9min 9min 9min 9mln 9mln 9min 9mln 9min . 9min 9min 9min 9min 9min 9mln 9min 9min 9mln 9mln 9mln B ottle 45 46 47 48 49 88 93 50 51 52 53 89 93 68 69 70 71 72 84 94 73 74 75 85 95 76 77 78 79 80 90 86 94 1. 2 3 4 5 6 7 8 9 10 11 000637 Masslynx Sample List Sample List: C:\MASSLYNX\rats2.PRO\SampleDB\042099d.SPL Printed: Tue Apr 2016:51:40 1999 - File Name 1 042099106 2 042099107 3 042099108 4 042099109 5 042099110 6 042099111 7 042099112 8 042099113 9 042099114 10 042099115 11 042099116 12 042099117 13 042099118 14 042099119 15 042099120 16 042099121 17 042099122 18 042099123 19 042099124 20 042099125 21 042099126 22 042099127 23 042099128 24 042099129 25 042099130 26 042099131 27 042099132 28 042099133 29 042099134 30 042099135 31 042099136 32 042099137 33 042099138 34 042099139 35 042099140 36 042099141 37 042099142 38 042099143 39 042099144 40 042099145 41 042099146 42 042099147 43 042099148 44 042099149 File Text MeOH Blank Tox120, RBL04199-H20Blk-1,4/19/99 Tox120, RBL04199-UvBlk-1,4/19/99 Tox120, RBL04199-5ppb-1,4/19/99 Tox120, RBL04199-10ppb-1,4/19/99 Tox120, RBL04199-25ppb-1,4/19/99 Tox120, RBL04199-50ppb-1,4/19/99 Tox120, RBL04199-100ppb-1,4/19/99 Tox120, RBL04199-250ppb-1, 4/19/99 Tox120, RBL04199-500ppb-1,4/19/99 Tox120, RBL04199-750ppb-1,4/19/99 Tox120, RBL04199-1000ppb-1,4/19/99 MeOH Blank Tox120, RTL, 49M, G 4 ,4/19/99 Tox120, RTL, 50M, G 4 ,4/19/99 Tox120, RTL, 51M, G 4 ,4/19/99 Tox120, RTL, 52M, G 4 ,4/19/99 Tox120, RTL, 53M, G 4 ,4/19/99 Tox120, RBL04199-250ppb-CC1,4/19/99 MeOH Blank Tox120, RTL, 54M, G 4 ,4/19/99. TOX120, RTL, 55M, G 4 ,4/19/99 Tox120, RTL, 56M, G 4 ,4/19/99 TOX120, RTL, 57M, G 4 ,4/19/99 Tox120, RTL, 58M, G 4 ,4/19/99 Tox120, RBL04199-250ppb-CC2,4/19/99 MeOH Blank Tox120, RTL, 59M, G 4 ,4/19/99 Tox120, RTL, 61 M, G 4 ,4/19/99 Tox120, RTL, 62M, G 4 ,4/19/99 Tox120, RTL, 63M, G 4 ,4/19/99 Tox120, RBL04199-250ppb-CC3,4/19/99 MeOH Blank . Tox120, RBL04199-H2OBIk-1,4/19/99 Tox120, RBL04199-UvBlk-1,4/19/99 Tox120, RBL04199-5ppb-1,4/19/99 Tox120, RBL04199-1Oppb-1,4 /1 9 /9 9 Tox120, RBL04199-25ppb-1,4/19/99 Tox120, RBL04199-50ppb-1,4/19/99 Tox120, RBL04199-1Q0ppb-1,4 /1 9 /9 9 ' Tox120, RBL04199-250ppb-1,4/19/99 Tox120, RBL04199-500ppb-1,4/19/99 Tox120, RBL04199-750ppb-1,4/19/99 Tox120, RBL04199-1000ppb-1,4/19/99 MS File Page 1 Inlet File long6 long6 long6 longe longe longe long6 longe long6 longe long6 long6 longe longe long6 longe long6 long6 longe long6 long6 long longe long6 longe long6 long6 long6 long6 long6 longe longe longe longe * longe " long6 long6 longe long6 long6 long6 long6 longe long6 ' Bottle 91 1 2 3 4 5 6 7 8 9 10 11 93 54 55 56 57 58 81 94 59 60 61 62 63 82 94 64 65 66 67 83 94 .1 2 3 4 5 6 7 8 9 10 11 000638 Masslynx - Sample List i Sample List: C:\MASSLYNX\rats2.PRO\SampleDB\042099d.SPL Printed: Tue Apr 2016:51:401999 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 40 41 42 43 44 File Name 042099106 042099107 042099108 042099109 042099110 042099111 042099112 042099113 042099114 042099115 042099116 042099117 042099118 042099T19 042099120 042099121 042099122 042099123 042099124 042099125 042099126 042099127 042099128 042099129 042099130 042099131 042099132 042099133 042099134 042099135 042099136 042099137 042099138 042099139 042099140 042099141 042099142 042099143 042099144 042099145 042099146 042099147 042099148 042099149 File Text MeOH Blank Tox120, RBL04199-H20Blk-1,4/19/99 Tox120. RBL04199-UvBlk-1,4/19/99 Tox120, RBL04199-5ppb-1,4/19/99 TOX120, RBL04199-10ppb-1,4/19/99 Tox120, RBL04199-25ppb-1,4/19/99 Tox120, RBL04199-50ppb-1,4 /1 9 /9 9 Tox120, RBL04199-100ppb-1, 4/19/99 Tox120, RBL04199-250ppb-1,4/19/99 Tox120, RBL04199-500ppb-1,4/19/99 TOX120, RBL04199-750ppb-1,4 /1 9 /9 9 Tox120, RBL04199-1000ppb-1,4/19/99 MeOH Blank TOX120, RTL, 49M, G 4 ,4/19/99 Tox120, RTL, 50M, G 4 ,4/19/99 Tox120, RTL, 51M, G 4 ,4/19/99 Tox120, RTL, 52M, G 4 .4/19/99 Tox120, RTL, 53M, G 4 ,4/19/99 TOX120, RBL04199-250ppb-CC1,4 /1 9 /9 9 MeOH Blank Tox120, RTL, 54M, G 4 ,4/19/99. Tox120, RTL, 55M, G 4 ,4/19/99 Tox120, RTL, 56M, G 4 ,4/19/99 Tox120, RTL, 57M, G 4 ,4/19/99 Tox120, RTL, 58M, G 4 ,4/19/99 Tox120, RBL04199-250ppb-CC2,4/19/99 MeOH Blank Tox120, RTL, 59M, G 4 ,4/19/99 Tox120, RTL, 61 M, G 4 ,4/19/99 Tox120, RTL, 62M, G 4 ,4/19/99 Tox120, RTL, 63M, G 4 ,4/19/99 Tox120, RBL04199-250ppb-CC3,4/19/99 MeOH Blank . Tox120, RBL04199-H2OBIk-1,4/19/99 Tox120, RBL04199-UvBlk-1,4/19/99 Tox120, RBL04199-5ppb-1,4/19/99 Tox120, RBL04199-1Oppb-1,4 /1 9 /9 9 Tox120, RBL04199-25ppb-1,4/19/99 Tox120, RBL04199-50ppb-1,4/19/99 Tox120, RBL04199-100ppb-1,4/19/99 ' Tox120, RBL04199-250ppb-1,4/19/99 Tox120, RBL04199-500ppb-1,4/19/99 Tox120, RBL04199-750ppb-1,4/19/99 Tox120, RBL04199-100Qppb-1,4 /1 9 /9 9 /K r Fagel / MS File 1 PFBS-4 PFBS-4 PFBS-4 PFBS-4 PFBS-4 PFBS-4 PFBS-4 PFBS-4 PFBS-4 PFBS-4 PFBS-4 PFBS-4 PFBS-4 PFBS-4 PFBS-4 PFBS-4 / PFBS-4 . PFBS-4 PFBS-4 I . PFBS-4 PFBS-4 PFBS-4 PFBS-4 PFBS-4 PFBS-4 PFBS-4 PFBS-4 PFBS-4 PFBS-4 PFBS-4 . PFBS-4 PFBS-4 PFBS-4 PFBS-4 PFBS-4 PFBS-4 i PFBS-4 \ PFBS-4 \ PFBS-4 \ PFBS-4 \ PFBS-4 \ PFBS-4 \ PFBS-4 \ PFBS-4 \ / / Inlet File longe long6 long6 long6 long6 long6 long6 long6 longe longe long6 long long6 long6 long6 longe long6 long6 long longe long6 long6 long6 long6 Iong6 longe long6 long longe long6 longe long6 long6 long long " long long6 long6 long long long long6 longe long6 Bottle 91 1 2 3 4 5 6 7 8 9 10 11 . 93 54 55 56 57 58 81 94 59 60 61 62 63 82 94 64 65 66 67 83 94 .1 2 3 4 5 6 7 8 9 10 11 000639 S e a m in g M ethod R a p e rt Method s C :\MASSLYHX\RATS2. 9RO\ACQUDB\9KBI-COMBX7ZS-PaAA L a s t `Modified: Toe A pr 20 16*33:12 1099 P rin te d * Tue A pr 20 16:33*19 1999 Solvent Delay ( nine ) s 0.00 Function * 1 KMC of 1 M a e Pair ( ESP- ) Inter Channel Delay ( Secs ) * Span ( Daltons ) s Start Tine ( Kins ) i Cnd Tine ( Mins ) ; Repeats * Channel Parent Daughter 0.03 0.00 0.00 9.00 1 Dwell (Secs) Coll Energy (eV) Cone { V ) 1 413.00 169.00 0.30 30 15 Function t 2 MRM of 1 Mass Pair ( ESP- ) Inter Channel Delay ( 5 . ) > Span ( Daltons ) : Start Time ( Mins ) x End Time ( Mins } i Repeats * Channel Parent Daughter 0.03 0.00 0.00 9.00 1 Dwell (Sees) . Cell Energy <.V) Cone 1 469.00 119.00 0.30 30 15 Function : 3 MSN of 1 Mass Pair ( ISP- ) Inter Channel Delay ( Secs ) i Span ( Daltons ) * Start Time ( Mins ) s End Tima ( Mins ) : Repeats : Channel Parent Dsughtsr 0.03 0.00 0.00 9.00 1 Dwell (Sees) Coll Energy (VI Cone 1 569.00 119.00 0.30 30 15 Function i 4 MRM of 1 Mass Pair ( ESP- ) Inter Channel Delay ( Secs ) : Span ( Daltons ) : Start Tine ( Mins ) t End T i m ( Mins ) : Repeats : Channel Parent Dsughtsr 0.03 0.00 0.00 9.00 1 Dwell (Secs) Coll Energy U V ) 1 419.00 119.00 0.30 30 Cone 15 Function : 5 MRM of 1 M u s Pair ( ESP- ) Inter Channel Delay ( Secs ) * Span { Daltons ) : Start T i m ( Mins ) : End T i m ( Mins ) : Repeats * Channel Parent Daughter 0.03 0.00 0.00 9.00 1 Dwsll (Sacs) Coll Energy (V) Cone 1 519.00 119.00 0.30 30 15 Function t 6 ' MRM of 1 Muse Pair ( ESP- ) Inter Channel Delay ( Sacs ) : Span ( Daltons ) t Start T i m ( Mins ) : End T i m ( Mins ) * Repests : Channel Parent Daughtar 0.03 0.00 0.00 9.00 1 Dell (Secs) Coll Energy (.V) Con. 1 499.00 9.00* 0.30 45 SO Function i 7 MSN of 1 Mase Pair < ISP- ) Inter Channel Delay ( Secs ) i -Span ( Daltons ) : Start Tiae ( Kina ') s End Tiae ( Mins ) I Repeats t Channel Parent Daughter 0.03 0.00 0.00 9.00 1 Dwell (Secs) Coll Energy (eV) Cone ( V ) 399.00 90.00 0.30 45 60 Function : S MSN of 1 Mass Pair ( ISP- ) Inter charnel Delay ( Secs ) i 0.03 Span ( Daltons ) 0.00 Start Tiae ( Mins ) : 0.00 End Tiae ( Mins ) i 9.00 Repeats * 1 Channel Parent Daughter Dwell (Secs) Coll Energy (eV) Cone ( V ) 1 427.00 90.00 0.30 40 90 Page 1 000640 S c a n n in g M athed R e p o rt Mathed: C:\WCJSLrNX\RAT92.PWJ\ACCMJ8\9MIM-C0KBma-FaAA last'Modifiad: Tua Apr 20 10:33:12 199 P rin ta d : tu a A pr 20 1 0 :3 3 :1 1999 P l 1 Solvant Dalay ( adna ) I 0.00 punetlon : 1 M M of 1 Maaa Pair ( ISP- ) Intar C h a m a l Dairy ( Seca ) t Span ( Daltons ) : Start Tina ( Hina ) End Tina ( Mina ) : Repasts : Channel Parent Daughter 0.03 0.00 0.00 9.00 1 Dwell (Saca) Coll Energy (V) Cona ( V ) 1 413.00 169.00 0.30 30 15 function i 2 MRM of 1 H u i Pair { ESP- ) Intar Channel Daisy ( Sees ) : Span ( Daltons ) I Start Tine ( Mina ) I End Tina ( Mina ) : Repeata : Charnel Parent Daughter 0.03 0.00 0.00 9.00 1 Dwell (Saca) Coll Energy (eV) Cona ( V ) 1 409.00 119.00 0.30 30 IS function t 3 MRM of 1 M m i Pair ( ESP- ) Inter Charnel Delay ( Secs ) x Span ( Daltons ) : Start Tine ( Mina ) : End Tina ( Mina ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 9.00 1 Dwell (Seca) Coll Energy (V) Cona ( V ) 1 509.00 119.00 0.30 30 IS / Function : 4 MRM of 1 Mill Pair < ESP- ) Inter Channel Deity ( Seca ) : Span ( Deltona ) : Start Tina ( Kina ) : End Tina ( Kina ) t Repeata x Channel Parent Daughter 0.03 0.00 0.00 9.00 1 Dwell (Seca) Coll Energy (V) Cona ( V ) 1 419.00 119.00 0.30 30 IS Funation 5 MRM of 1 M u i Pair ( ESP- ) Inter Channel Delay ( Seca ) t Span i Daltona ) : Start Tiae ( Mins } i End Tiae ( Mins ) t Repeata i Channel Parent Daughter 0.03 0.00 0.00 9.00 1 Dwell (Seca) Coll Energy (V) Cona ( V J 1 519.00 119.00 0.30 30 15 A Function x * MRM of 1 Maaa Pair ( ESP- ) Inter Channel Delay ( Seca ) t Span ( Daltona ) : Start Tine ( Mina ) : End Tine ( Mins ) : Repeats s Channel Parent Daughtar 0.03 0.00 0.00 9.00 1 Dwell , (Seca) Coll Energy (V) Cona ( V ) 1 499.00 99.00* 0.30 45 00 Funation x 7 MRM of 1 Mese pair ( BSP- ) Inter Channel Delay { Secs ) x Span t Daltona 1 s Start Tine ( Mina *) : End Tine ( Mins } i Repeats t Channel Parent Daughter 0.03 0.00 0.-00 9.00 1 Dwell (Saca) Coll Energy (V) Cona [ V ) 1 - 399.00 80.00 0.30 45 00 Function x 8 MRM of 1 Maas Pair ( ISP- ) Inter Channel Delay ( Sec* ) i Span | Daltona ) : Start Tine ( Hina ) t End Tine < Mina ) x Repeats i Channel Parent Daughter 0.03 0.00 0.00 9.00 l Dwell (Saca) Coll Energy (V) Cona ( V ) 1 427.00 90.00 0.30 40 00 000641 canning Method Xaport Method: C:\HASSUna\RAM2.PII0VACaD0B\ LS Modified: Mon Mar 15 14:22:03 1999 P rin te d : Tua A pr 20 1 7 :0 5 :2 p 1P9P -4 Solvant Delay ( nina 1 t 0.00 function t X KRK of 4 K u i Padre ( ISP- ) Inter Channel Delay ( Seca > : Span ( Daltona ) : Start Tina (.Mina ) End Tina ( Mina ) : Rapaata : Channel Parent Daughter 0.03 0.00 0.00 13.50 1 Dwell (Saca) Coll Energy (eV) Cone.< V ) 1 299.00 '90.00 0.30 2 299.00 99.00 0.30 3 299.00 130.00 0.30 4 299.00 180.00 0.30 45 45 45 45 60 60 60 60 1 T ] ii I j J J ] ] I j i ' \ 4 Paga 1 n. 000642 AM ELIA062498: FACT E quipm ent L og 99016 Q uattro H , #6448E PAGE DATE: 04/22/99 ANALYST: mee STUDY NUM BER Tox-120 M ATRIX: R at L iver D ESCRIPTION: ip FACT M ethod: ETS-8-5.0________ Injection volum e. IO uL C ycle tim e: 13.5 m in. M obile P hase: (AYLO m M NH4CH3CQ2 TN-A- or stndrd num ber (A ) 99012-5-22_________ Prepared (date/by): (A) 4/16/99 / ok_________ Expires: (A ) 10/99________________ Electrode: Z-Spray (B) M eOH (B) TN-A-2414 (B ) 4/9/99 hoi IB ) 10/99________ Store at room tem p? [YJ or N O ther G u ard colum n: N one ______________ _ Part number: na_________ L ot num ber: na A nalytical colum n: keystone betasil____________________________________________ Size: 2 x 50mm__________________ Type: c l 8____________ Sphere size: 5 um P art number: 055-701-2 L ot num ber: P7L04 Serial num ber 0481172z A nalytical p aram eters: t Drying gas (L/hr): 300 ESI nebulizing gas (L/hr) 15 LC Flow rate: 300 uL/m in. B ack pressure: 59 b ar '' H PLC solvent g rad ien t: long2 Tim e (m in.) 1) 0.00________ 2) 8.5__________ 3 11.0________ 5) 12.0________ 6) 13.5_________ %B 40 90 90 40 stop Sheath gas (L/hr) 0 .*s. 000(b43 AM ELIA062498: FACT E quipm ent Log 99016 Q uattro II, #6448E P A G E ________ DATE: 04/22/99 ANALYST: mee STUDY NUM BER Tox-120 M ATRIX: R at L iver (pfbs) DESCRIPTION: ip FACT M ethod: ETS-8-5.0 Injection volum e.10 uL C ycle tune: IS m in. Electrode: Z-Spray MobUe P hase: (A12.0 mM NH4CH3CQ2 TN-A- or stndrd num ber (A) 99012-5-22 Prepared (date/by): (A) 4/16/99 / ok Expires: (A ) 10/99 (B) MeOH (B ) TN-A-2414 (B) 4/9/99 hoi (B ) 10/99 Store at room temp? (Y| or N O ther: G u ard colum n: None _________ Part number, na L ot number: na A nalytical colum n: keystone betasil________________ _________________ Size: 2 x 50mm_________________ Type: c l 8 __________ Sphere size: 5 urn Part number: 055-701-2 Lot number: P7L04 Serial num ber: 0481172z A nalytical param eters: Drying gas (L/hr): 300 ESI nebulizing gas (L/hr) 15 LC Flow rate: 300 uL/m in. B ackpressure: 59 bar Sheath gas (L/hr) 0 H PLC solvent g rad ien t: long2 Time (m in.) 1) 0.00________ 2) 5.0__________ . 3 12.0 51 13.5 6) 15_________ %B 25 95 95 25 stop 000644 /^ fZ F Tuning Method Report Method: C:\MASSLYNX\RATS2.PR0\ACQUDB\PF0S Printed: Thu Apr 22 16:25:24 1999 AimL OLiHHf Page 1 LAC, Of/l/M BESTCOPYAVAILABLE SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. Set Rdbk 3.00 15 5 0.2 150 250 2.96 -14 -5 - 152 253 Pressures Analyser Vacuum Gas Cell Rdbk 2. Oe-4 5 . 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 . 58 650 Set Rdbk 15.0 15.0 30 2.0 0.0 40 0 650 32 39 31 000645 Masslynx - Sample List Sample List: C:\MASSLYNX\rats2.PRO\SampleDB\042299a.SPL Printed: Thu Apr 2217:50:31 1999 ^ y/*<;?7 Page 1 File Name File Text 1 042299001 MeOH Blank 2 042299002 Tox120, RBL04199-H 20Blk-1,4 /1 9 /9 9 3 042299003 TOX120. RBL04199-LivB!k-1,4/19/99 4 042299004 Tox120, RBL04199-5ppb-1,4/19/99 5 042299005 TOX120, RBL04199-10ppb-1,4/19/99 6 042299006 OX120, RBL04199-25ppb-1,4/19/99 7 042299007 TOX120, RBL04199-50ppb-1,4 /1 9 /9 9 8 042299008 TOX120, RBL04199-1 OOppb-1,4/19/99 9 042299009 Tox120. RBL04199-250ppb-1,4 /1 9 /9 9 10 042299010 TOX120, RBL04199-500ppb-1,4 /1 9 /9 9 11 042299011 TOX120, RBL04199-750ppb-1,4 /1 9 /9 9 12 042299012 Tox120, RBL04199-1000ppb-1,4/19/99 13 042299013 MeOH Blank 14 042299014 TOX120, RTL, 49M, G 4 ,4/19/99, D10 15 042299015 TOX120, RTL, 50M, G 4 ,4/19/99, D10 16 042299016 TOX120, RTL, 51M, G 4 ,4/19/99, D10 17 042299017 Tox120, RTL, 52M, G 4 ,4/19/99, D10 18 042299018 Tox120, RTL, 53M, G 4 ,4/19/99, D10 19 0422990-19 TOX120, RBL04199-250ppb-CC1,4 /1 9 /9 9 . 20 042299020 MeOH Blank 21 042299021 TOX120, RTL, 54M, G 4 ,4/19/99, D10 22 042299022 TOX120, RTL, 55M, G 4 ,4/19/99, D10 23 042299023 Tox120, RTL, 56M, G 4 ,4/19/99, D10 24 042299024 Tox120, RTL, 57M, G 4 ,4/19/99, 25 042299025 TOX120, RTL, 58M, G 4 ,4/19/99, 26 042299026 TOX120, RBL04199-250ppb-CC2,4/19/99 27 042299027 MeOH Blank 28 042299028 Tox120, RTL, 59M, G 4 ,4/19/99, 29 042299029 TOX120, RTL, 61 M, G 4 ,4/19/99, 30 042299030 TOX120, RTL, 62M, G 4 ,4/19/99, . 31 042299031 TOX120, RTL, 63M, G 4 ,4/19/99, 32 042299032 TOX120, RB L04199-250ppb-CC1,4 /1 9 /9 9 33 042299033 MeOH Blank 34 042299034 TOX120, RBL04199-H2OBIk-1,4/19/99 35 042299035' TOX120, RBL04199-LlvBlk-1,4 /1 9 /9 9 36 042299036 Tox120, RBL04199-5ppb-1,4/19/99 37 042299037 TOX120, RBL04199-1 Oppb-1,4 /1 9 /9 9 38 042299038 . TOX120, RBL04199-25ppb-1,4/19/99 39 042299039 T0 X I2 O, RBL04199-50ppb-1,4/19/99 40 042299040 TOX120, RBL04199-100ppb-1,4/19/99 41 042299041 TOX120, RBL04199-250ppb-1,4/19/99 42 042299042 TOX120, RBL04199-500ppb-1,4 /1 9 /9 9 43 042299043 Tox120, RBL04199-750ppb-1,4/19/99 44 042299044 TOX120, RBL04199-1000ppb-1,4/19/99 > MS File 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15M1N 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15MIN 15M1N 15MIN 15MIN 15MIN Inlet R e long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 * long15 long15 long15 long15 long15 long15 long15 long15 long15 long15 Bottle 91 1 2 3 4 5 6 7 8 9 10 11 91 12 13 14 15 16 17 91 18 19 20 21 22 23 91 24 25 26 27 17 92 1 .. 2 3 4 5 6 7 8 9 10 11 000646 VA*Jw Masslynx - Sample List Sample List: C:\MASSLYNX\rats2.PRO\SampleDB\042299b.SPL Printed: Thu A p r2217:46:29 1999 ____________ / W i f f l . b L M H # I A C 6.ilh d tf . Page 1 File Name File Text 1 042299045 MeOH Blank 2 042299046 Tox120, RBL04199-H20B!k-1,4/19/99 3 042299047 Tox120, RBL04199-LivBlk-1,4/19/99 4 042299048 Tox120, RBL04199-5ppb-1,4/19/99 5 042299049 . Tox120, RBL04199-10ppb-1,4/19/99 6 042299050 Tox120, RBL04199-25ppb-1,4/19/99 7 042299051 Tox120, RBL04199-50ppb-1.4/19/99 8 042299052 TOX120. RBL04199-100ppb-1,4 /1 9 /9 9 9 042299053 Tox120, RBL04199-250ppb-1, 4/19/99 10 042299054 Tox120, RBL04199-500ppb-1,4/19/99 11 042299055 Tox120, RBL04199-750ppb-1,4/19/99 12 042299056 Tox120, RBL04199-1000ppb-1,4/19/99 13 042299057 MeOH Blank 14 042299058 Tox120, RTL, 17M, G 2 ,4/19/99 15 042299059 Tox120, RTL, 18M, G 2 ,4/19/99 16 042299060 Tox120, RTL, 19M, G 2 ,4/19/99 17 042299061 Tox120, RTL. 20M, G 2 ,4/19/99 18 042299062 Tox120, RTL. 21M, G2. 4/19/99 19 042299063 Tox120, RBL04199-250ppb-CC4,4/19/99 . 20 042299064 MeOH Blank 21 042299065 Tox120, RTL, 22M, G 2 .4/19/99 22 042299066 Tox120, RTL, 23M, G 2 ,4/19/99 23 042299067 Tox120, RTL, 24M, G 2 ,4/19/99 24 042299068 Tox120, RTL, 25M, G 2 ,4/19/99 25 042299069 Tox120, RTL, 26M, G 2 ,4/19/99 26 042299070 Tox120, RBL04199-250ppb-CC5,4/19/99 27 042299071 MeOH Blank 28 042299072 Tox120, RTL, 27M, G 2 .4/19/99 29 042299073 Tox120, RTL, 29M, G 2 ,4/19/99 30 042299074 Tox120, RTL, 30M, G 2 ,4/19/99 31 042299075 Tox120, RTL, 31 M, G 2 ,4/19/99 32 042299076 Tox120, RBL04199-250ppb-CC6,4/19/99 33 042299077 MeOH Blank 34 042299078 Tox120, RTL, 33M, G 3 ,4/19/99 35 042299079 Tox120, RTL, 34M, G 3 ,4/19/99 36 042299080 Tox120, RTL, 35M, G 3 ,4/19/99 37 042299081 Tox120, RTL, 36M, G 3 .4/19/99 38 042299082 Tox120, RTL, 37M, G 3 ,4/19/99 39 042299083 Tox120, RBL04199-250ppb-CC7,4/19/99 40 042299084 MeOH Blank 41 042299085 Tox120, RTL, 38M, G 3 ,4/19/99 42 042299086 Tox120, RTL, 39M, G 3 ,4/19/99 43 042299087 Tox120, RTL, 40M, G 3 ,4/19/99 44 042299088 TOX120, RTL, 41M. G 3 .4/19/99 45 042299089 Tox120, RTL, 42M, G 3 ,4/19/99 46 042299090 Tox120, RBL04199-250ppb-CC 8,4/19/99 47 042299091 MeOH Blank 48 042299092 Tox120, RTL, 43M, G 3 ,4/19/99 49 042299093 Tox120, RTL, 45M, G 3 ,4/19/99 50 042299094 Tox120, RTL, 46M, G 3 ,4/19/99 51 042299095 Tox120, RTL, 47M, G 3 ,4/19/99 52 042299096 Tox120, RBL04199-250ppb-CC9, 4/19/99 53 042299097 MeOH Blank 54 042299098 Tox120, RB L04199-H20Blk-1, 4/19/99 55 042299099 Tox120, RBL04199-LivBIk-1, 4/19/99 56 042299100 Tox120, RBL04199-5ppb-1,4/19/99 57 042299101 Tox120, RBL04199-1 Oppb-1,4 /1 9 /9 9 58 042299102 Tox120, RBL04199-25ppb-1, 4/19/99 59 042299103 Tox120, RB L04199-50ppb-1, 4/19/99 60 042299104 Tox120, RBL04199-100ppb-1, 4/19/99 MS File Inlet File 13MIN-COMBI7IS-POAA 13MIN-COMBI7IS-POAA 13 M IN -C O M B I7 IS -P O A A 13MIN-COMBI7IS-POAA 13MIN-COMBI7IS-POAA 13MIN-COMBI7IS-POAA 13MIN-COMBI7IS-POAA 13M IN-COM BI7IS-POM 13MIN-COMBI7IS-POAA 13MIN-COMBI7IS-POAA 13MIN-COMBI7IS-POAA 13 M IN -C O M B I7 IS -P O A A 13 M IN -C O M B I7 IS -P O A A 13MIN-COMBI7IS-POAA 13 M IN -C O M B I7 IS -P O A A 13 M IN -C O M B I7 IS -P O A A 13MIN-COMBI7IS-POAA 13 M IN -C O M B I7 IS -P O A A 13M IN-COMB I7IS-POAA 13MIN-COMBI7IS-POAA 13MIN-COMBI7IS-POAA 13M IN -C O M B I7IS -P O M 13MIN-COMBI7IS-POAA 13MIN-COMBI7IS-POAA 13MIN-COMBI7IS-POAA 13MIN-COMBI7IS-POAA 13MIN-COMBI7IS-POAA 13MIN-COMBI7IS-POAA 13 M IN -C O M B I7 IS -P O A A 13M IN-COMB I7IS-POAA 13 M IN -C O M B I7 IS -P O A A 13MIN-COMBI7IS-POAA 13MIN-COMBI7IS-POAA 13 M IN -C O M B I7 IS -P O A A 13 M IN -C O M B I7 IS -P O A A 13MIN-COMBI7IS-POAA 13 M IN -C O M B I7 IS -P O A A 13MIN-COMBI7IS-POAA 13 M IN -C O M B I7 IS -P O A A 13MIN-COMBI7IS-POAA 13MIN-COMBI7IS-POAA 13 M IN -C O M B I7 IS -P O A A 13MIN-COMBI7IS-POAA 13 M IN -C O M B I7 IS -P O A A 13MIN-COMBI7IS-POAA 13MIN-COMBI7IS-POAA 13M IN -C O M B I7 IS -P O A A 13MIN-COMBI7IS-POAA 13MIN-COMBI7IS-POAA 13MIN-COMBI71S-POAA 13MIN-COMBI7IS-POAA 13MIN-COMBI7IS-POAA 13 M IN -C O M B I7 IS -P O A A 13 M IN -C O M B I7 IS -P O A A 13 M IN -C O M B I7 IS -P O A A 13MIN-COMBI7IS-POAA 13MIN-COMBI7IS-POAA 13MIN-COMBI7IS-POAA 13 M IN -C O M B I7 IS -P O A A 13 M IN -C O M B I7 IS -P O A A long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 tong2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 Iong2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 long2 Bottle 91 1 2 3 4 5 6 7 8 9 10 11 91 31 32 33 34 35 84 92 36 37 38 39 40 85 92 41 42 43 44 86 93 45 46 47 48 49 87 93 50 51 52 53 54 88 93 55 56 57 58 89 93 1 2 3 4 5 6 7 000647 Masslynx * Sample List Sample List: C:\MASSLYNX\rats2.PRO\SampleDB\042299b.SPL / Printed: Thu Apr 2217:46:291999______________________ A m l i C . File Name 61 042299105 62 042299106 63 042299107 64 042299108 65 66 67 68 70 71 72 73 74 File Text Tox120, RBL04199-250ppb-1,4/19/99 Tox120, RBL04199-500ppb-1,4/19/99 TOX120, RBL04199-750ppb-1,4 /1 9 /9 9 Tox120, RBL04199-1000ppb-1,4/19/99 y /* < ./? y Page 2 /, I A D / Z o / ^ _______________ M S File 13M1N-COMBI7IS-POAA 13M1N-COMBI7IS-POAA 13 M IN -C O M B I7 IS -P O A A 1 3 M IN -C O M B I7 IS -P O A A Inlet File long2 long2 long2 long2 Bottle 8 9 10 11 000648 V /^ v 9 / c a n n in g M ethod R a p o rt Mathod: C!\MASSLWX\ItATSa.P0\ACQUDB\13MXH-CCt<BI7I-PQAA taut Modified: Thu Apr 22 1C:S0:10 1999 Printed: Thu Apr 22 1:30:1( 1999 A p v L ____n u x i V Solvant Delay ( nine ) i 0.00 Punction : X to o f 1 Mfeaa fair { ESP- ) Inter Channel Delay ( Seca 1 t Span ( Daltons I ; Start Tine ( Kins 1 : End Tine ( Kins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 13.50 1 Dwell (S.ca) Coll Energy (eV) * Co m ( V ) 1 413.00 169.00 0.30 30 15 function : 2 MRM of 1 Maes fair I ESP- ) Inter Channel Delay ( Saca ) : Span ( Daltons ) : Start Time | Hina ) ! End Tine l Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 13.50 1 Dwell , (Saca) Coll Energy (aV) 1 469.00 119.00 0.30 45 * Cone C V ) 33 function : 3 MRM of 1 Haai Pair ( ESP- ) Inter Channel Delay ( Saca ) : Span ( Daltons ) : Start Time ( Mina ) : End Tine ( Mins ) : Repeats i Channel Parent Daughter 0.03 0.00 0.00 13.50 1 Dwell (Saca) Coll Energy (eV) COM t V > 1 569.00 119.00 0.30 45 35 function : 4 MRM of 1 Mass Pair t ESP- ) Inter Channel Delay ( S.ca ) i Span ( Daltons ) : Start Tine ( Mins ) : End Tine ( Mins ) s Repeats t Channel Parent Daughter 0.03 0.00 0.00 13.50 1 Dwell (Saca) Coll Energy (aV) . Cone ( V ) 1 419.00 119.00 0.30 45 35 function : 9 MRM of 1 Miss fair { ESP- ) Inter Channel Delay ( S.ca ) : Span ( Daltons ) : Start Tine { Mina ) : End Tim. ( Mina ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 13.50 1 Dwell (Secs) Coll Energy (eV) Cone ( V ) 1 519.00 119.00 0.30 45 35 Function : ( ' MRM of 1 Maaa Fair { ESP- > Inter Channel Delay ( Saca ) Span ( Daltons ) : Start Tine { Mins ) : End Tine J Mins ) ; Repeats : Channel Parent Daughter 0.03 0.00 0.00 13.50 1 Dwell (S.ca) Coll Energy (V) Cano ( V ) 1 499.00 99.00* 0.30 45 <0 function t 7 MRM of 1 Maas fair ( ESP- ) Inter Channel Delay ( Secs ) i Span ( Daltona ) Start Tim* ( Mina ) i End Tine ( Mina ) t Repeats s Channel Parent Daughter 0.03 0.00 0.00 13.50 1 Dwell (Secs) Coll Energy (eV) 1 399.00 60.00 0.30 45 Cone I V 1 <0 Function : S MRM of 1 Maaa fair ( ESP- ) Intar Channel Delay ( Secs ) ; Span ( Daltons ) : Start Tine { Mins ) s End Tine ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 13.50 1 Dwell (Secs) Coll Energy (V) 1 427.00 80.00 0.30 40 Cone ( V ) 60 LAc- o i L h t .t* 000649 P ig t 1 S c a n n in g M ethod R e p o rt Method: c:\MMSLnoc\iuTS2.MoVAOQOoaUSK Last Modifiad: Thu Apr 32 13:32:50 1999 Printed: Thu Apr 22 13:52:34 1999 Solvent Dlay < nine > > 0.00 function : 1 M M a t 4 Mass fairs ( U f - 1 Inter Channel Delay (1 Sac* ) i Span ( Daltons ) : Start Tine ( Kina ) i End Tine ( Mine J : Repeats s Channel Parent Daughter 9.03 0.00 0.00 IS.00 1 Etoell (Secs) 1 299.00 90.00 0.30 2 299.00 99.00 0.30 a 299.00 130.00 0.30 4 299.00 180.00 0.30 45 45 45 45 1 i I sH* A n u L /LVIV Ucox/io/w Cons | V J 60 60 60 60 fag s 1 000650 S c a n n in g M ethod R e p o rt Hathod: C: \ M M a L 0 ( \ R X I S .P0\*CQUI!B\1 Last Modified: Ihn Apr 22 19:92:90 1* Prlntad: Thu Apr 22 19:92:94 199 ________ ri rmr i ttt iLfj n h W Solvant Palay ( atina )i i 0.00 function : 1 m M of 4 Haas falsa ( IIP- > Intar Charmai Palay ( Sacs ) : Span ( Daltons ) : Start Tiaa ( Hina ) : End Tina { Kina ) : Riputa : Channel Parant Daughtar 0.03 0.00 0 a00 19.00 1 thrall (Secs) Coll Energy (aV) Cons I V ) 1 299.00 90.00 0.30 2 299.00 99.00 0.3 3 299.00 130.00 0.30 4 299.00 190.00 0.30 45 45 45 45 60 60 60 60 * //* * /? ? Pag. i U t O j/z o /w er 000651 ] FACT: DATA REVIEW SUMMARY FORM Date: 4 /2 3 /0 9 ] Analyst: L FACT Study Number 1 D X - 1 ^ 0 I Matrix \A a d jL U ' w f Urne Points 1 Dilutions? tffu p H S(/mc oaJ - 3 Analyte 1: fNr..p...b...s^'i Acceptable LinearRange: 1 ipnplo LOQ fiartills data set: 1 Reevahuted&r differentname? fvo Analyte 4: Acceptable Linear Ranjg: LOQ for this data set Reevaluated for different Analyte 5: Acceptable] LOQfor tbia data set Lfor dxffbicQ-trange? Analyte2: Acceptable LinearRango: LOQ far this data set ] Reevaluated for different range? J Analyte3; Acceptable Linear Range: LOQ fiartills data set 3 Reevaluated for differentrange?, z A j l y t e 6: Acceptablelinear Range: A \ LOQ for this data set Reevaluated for differentrange? Analyte 7: Acceptable T Range: LOQfor tide data set: Reevaluated far different range? ] DinJfilU potk* * dkAJXKSi- j \oof*. p*-ab* i'oprJr*d- i V U '5 o. (yu * f / 2 - 5 / d 3 J ] 000652 i FACT: DATA REVIEW SUMMARY FORM Date: Analyst: FACT Study Number JL T V X 'IU ) Matrix Tima Pointa Dilutions? h a lt u m v s m c p y- SU Y ru. yy X~ Analyte 1: Acceptable LinearRange: 5 '^ 7'S D lr> jylo LOQ for ds data set: Re-evahiated far differentrange? oo Analyte 2: Acceptable LinearRange: LOQ for this data set Re-evaluated for differentrange? Analyte 3; Acceptable Linear Rango^ LOQ for this data set Re-evaluated for differentrange? Analyte 4: Acceptable Linear Range: LOQ for this data set: Re-evaluated for different Analyte 5: Acceptable LOQ for this i&ta set: Acceptable Linear Range: LOQ for this data set Re-evaluated for differentrange? Analvte7: Acceotable Linear Range: LOOfor this data set Re-evaluated for different range? X )o J fiU p u d * -*'* \} M S O -. fcp. . 000653 Vi o 1 Vt0VO*Bil)iO HHN I I CM III t SS522SSSSSisSliS5SS55SiSSS3SSSS2S:8SSSS )nH rn >*ioHrv ri A* r'oo'n no on iHv h< ,St Hn Hi rn'B*ODrr4f ) Di fw lfrtaw*snoMin >9 )r a noviNnnSHM Hn t oN <anenr*NrHH n HrHt N h s NMSS^HB Pv tvnNvSnO N Hi oBfO BH elfNtrN'Oi Nn vhoiflfftHN Bn vNotHo if tnviABMn^oooA h n o n n rt f N l O ^ rr t rt r* n w kjh n h t h t * nr* r* >nnmnMSSiNnw^pS*f^nSnBaCInmSoS^tS'SoS~lorovthOfH*Atow^rHvrSnVrtOS-OMSr-e'moi-D<Shrf l a w m a h v D f - n n o N h HNnHNV H W w n HHi tT0i N H H H r * H N D H h hHn Ht J^AOMNxAAnwAaAArnrtA"AntAnf'*tn*nio,nooxnff*'imerW*nNrnWA^Nrr'N*AAiMXniHr-lM*NrrNrNr'*iNo*'B0f'*oi^nnow'AnOMo^ inr-frnl*ran%NrANfo,>fsAn*n0nMsn,aAnanrsn*sAn fsn-snA lo n o o o o o o HNinomomo -tenor o litllllif M oweooooo HMSoaomo HNlflhO ikhhhN M M h ilfiillil Last nodifitdi ftl Apr 23 08:42:43 1999 C:\MfcS9LTOC\rata2.FRO\MathDB\042299a Last nodlfiad: M Apr 23 08:51:2 199 arpia List: C :\MfcSSLYXX\rt*2.PRO\SawplaDB\042299a .NOAkAASafAtAAAAASANAAANAANA'sA. AAs ooooos H H H H pt A QOOQQh ooo H H p< QQ NHAANHANA'AH>AH.NAH.HASANHANrtAHNiHS^ SAHNAHSAr-tSpA1.SAHUO AAAAAAAA sAAHAsAAHAaAN'asA.a-Af^tA'AAs.AAHsAAAsHAAsAHAAsAHAAV-V. PV W NAH SHASHASHA.UHU .H H HH I I I .HH H I I I I A 3 3VAAS||S ghfhaasosmao&oAUoSmso V.^. X.1.^ ^*Qi .. ^ r . .. r ^ a o oo u o litn u o u u o m o>ftftftftoooooN N^ S S AI I I .H H H I M M r * l I I 4343A._ as * A* n o i l 'S a 'S. f t'Sa-Sa ' f to ^^ ^o ooeum ftonooinom o SdflHN ArtN flr>H BZU ooooooooooo %%o ..*;..O ***JO oooooocAI AI AI AI AI AI Ai Al AIAI AI AAAAAAAAAAA SS5SSS .I &388 tt AAAAAAAAAAA oooo 1*4 J 1a |^S2SSSS2SaSS3SEa|SSS3S|SaS2S2! 2222 u SrlX"ofaHXtn*OoHXn--O-o-HXn-O-o--HXn-O-o-H-Xn-O-o*HXnO*oHnX*OoHnXiOoHInXOpHnXOonXOoOAaXnOoXnOoXOoXnOoXnOo XOo OA_a XOno XiO*onXO*onXO*onXOw*o XOo.n...O.A._a....XO.o....XO.om....O.o.X...O.oX.n..OonXAOOp*nXOpnHXOpnHXOnpHXnOoHXmOoHXONHXo HONXo HONoXHONoXHOnoX ooeo3INNHoAoAWNHNAAoo NN-NAoAo.MHNAAoo.NN<ANooANNnNNXAAoowNNNNAooAr>NNNNAAooNNNXAoAAoNNAANXOWNMNAAONNAANNOWNNOAAMNNAnBoaNHNNtnNAeaHNlNMonAaHNvMnoAaNHNrnoANaHWBnoAManHMnoAAONNNnoHAANNNnnoAaPNNNrnloAaNNiNnAoANvNNnAoaNBNNnAoaWNNNnAoMaNNNniAoaNNNBnAoaNNONnAoaNNinnAoafNNirlnAoatNNWNnwaAoNnnNNnAANoWHCAAorMiWNNAANpoNNi[NNAAon'NNNAoAni>IINN(fnOnAAN<0<rWNoAOVNAHANANONNANOANNAA^On--NNOA^At S Ho No no o so o No so AoOoHoNonoio o o o o o o o o o o o o o o o o o o o o o o o o o o Job Coda: Hsthod: U CD O O O A m i l a 042498; Raviawad and quanti tatad by kjh 4/23/99 Quantify Calibration Raport Calibration: C:\HAS3Un0C\rata2.PRO\CurvaDB\042299a Last aodifiad: Fri Apr 23 08:31:34 1999 Printad: Pri Apr 23 08:32:40 1999 ' Pag 1 Amalia 082498: Raviawad and quantitatad by kjh 4/23/99 000655 000656 1 ;p O e $ ? 1*0 -t Mt (titHH er H tu `tNnttMa<(i*NS'<>tn tiM i ii ** ti{M i\u wn itvi nm m SOUP 020199: FACT Equipm ent L og 99014 Q uattro II, #6414E PAGE DATE: 05/14/99 A N A L Y S T idrb STUDY NUMBER: T ox-120 M ATRIX: R at Liver DESCRIPTION: dilutions, FACT M ethod: ETS-8-S.0 . Injection volume: 10 uL Cycle tim e: 9 min. Electrode: Z-Spr^y--------- M obile P hase: (A12.0 mM NH4CH3CQ2 (B)M eQ H --------- TN-A- or stndrd num ber (A) 99011-6-9__________ (B) TN-A-25.Q6 Prepared (date/by): fAl 04/28/99 drb______ _ (B) Q4/26/99,drb Expires: (A1 10/99_____________ __ (B ).,10/99_____ Store at room temp? [y| or N Other:---------------------------- .-------- G u ard colum n: None______________ P art number: na_________ Lot num ber:jna_______________________ A nalytical colum n: Keystone B etasil __________________________________ Size: 2 X 50 mm ___________ Type:j18____________ Sphere size:J u ffi______ Part number: 055-701-2__________ L ot num ber P7LQ4 Serial numben0481175Z A nalytical param eters: Drying gas (L /hrl: 350 ESI nebulizing gas (L/hrl 15 LC Flow rate: 3 0 0 11T./min. B ack pressure: 55 bar Sheath gas (L/hr)^. H PLC solvent gradient: 9m in-2 Time (min.) D0.00______ 2) 1.00______ 3) jL5Q____ 416.50 51 7.00______ %B_ 40.0 40.0 J10 35SL 40.0_ 000657 Tuning Method Report Method: C :\MASSLYNX\KACT-1.PRO\ACQUDB\PFOS Printed: Pri May 14 16:17:39 1999 Rage 1 .EST COPY AVAILABLE MS SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. Set Rdbk 3.00 60 5 0.2 150 250 2.98 -29 -7 153 248 Pressures Analyser Vacuum Gas Cell Rdbk 3.3e-5 4 .3e-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier '.*X MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set Rdbk 14.0 14.0 * 2.0 . 0.0 56 650 Set Rdbk 15.0 15.0 45 2.0 0.0 40 0 650 42 40 44 000658 Masslynx - Sample List Sample Ust: C:\MASSLYNX\FACT-1.PRO\SampleDB\05T499c.SPL Printed: Fri May 1416:17:21 1999 Page 1 File Nami File Text MS R ie Inlet I Botti ilume Sample T Cone A 1 05149906 MeOH Blank 2 05149906 MeOH Blank 3 05149906 Tox-120, RBL04199-H20Blk-2,4/19/99 4 05149906 Tox-120, RBL04199-LBIk-2,4/19/99 5 05149906 Tox-120, RBL04199-5ppb-2,4/19/99 6 05149906 Tox-120, RBL04199-10ppb-2, 4/19/99 7 05149906 Tox-120, RBL04199-25ppb-2,4/19/99 8 05149906 Tox-120, RBL04199-50ppb-2, 4/19/99 9 05149906 Tox-120, RBL04199-1 OOppb-2,4/19/99 10 05149907 Tox-120, RBL04199-250ppb-2,4/19/99 11 05149907 Tox-120, RBL04199-500ppb-2,4/19/99 12 05149907 Tox-120, RBL04199-750ppb-2,4/19/99 13 05149907 Tox-120, RBL04199-1000ppb-2, 4/19/99 14 05149907 MeOH Blank 15 05149907 Tox-120 23M G 2/D 1:25 16 05149907 Tox-120 24M G2 / D1:25 17 05149907 Tox-120 25M G2 / D1:25 18 05149907 Tox-120 26M G 2/D 1:25 19 05149907 Tox-120, RBL04199-250ppb-CC1, 4/19/99 20 05149908 MeOH Blank 21 05149906 Tox-120 33M G 3 /D 1 2 5 22 05149908 Tox-120 34M G3/D1 5 23 05149908 Tox-120 35M G 3/D 1:25 24 05149908 Tox-120 36M G 3/D 1:25 25 05149908 Tox-120 37M G 3/D 1:25 26 05149908 Tox-120 38M G 3 /D 1 2 5 27 05149908 Tox-120 39M G 3/D 1:25 28 05149908 Tox-120 40M G 3/D 1:25 29 05149908 Tox-120, RBL04199-250ppb-CC3,4/19/99 30 05149909 MeOH Blank 31 05149909 Tox-120 2 7 M G 2 /D 1 :1 0 32 05149909 Tox-120 2 9 M G 2/D 1:10 33 05149909 Tox-120 30M G 2/D T.10 34 05149909 Tox-120 31 M G 2 /D 1 :1 0 35 05149909 Tox-120, RBL04199-250ppb-CC4, 4/19/99 36 05149909 MeOH Blank 37 05149909 Tox-120 4 2 M G 3/D 1:10 38 05149909 Tox-120 43M G 3/D 1:10 39 05149909 Tox-120 45M G 3/D 1:10 40 05149910 Tox-120 46M G 3/D 1:10 ' 41 05149910 Tox-120 4 7 M G 3 /D 1 :1 0 42 05149910 Tox-120, RBLQ4199-250ppb-CC5, 4/19/99 43 05149910 MeOH Blank 44 05149910 Tox-120, RBL04199-H20Blk-2, 4/19/99 45 05149910 Tox-120, RBLQ4199-LBIk-2,4/19/99 46 05149910 Tox-120, RBL04199-5ppb-2,4/19/99 47 05149910 Tox-120, RBL04199-1 Oppb-2,4/19/99 48 05149910 Tox-120, RBL04199-25ppb-2,4/19/99 49 05149910 Tox-120, RBL04199-50ppb-2,4/19/99 50 05149911 Tox-120, RBL04199-1 OOppb-2,4/19/99 51 05149911 Tox-120. RBL04199-250ppb-2,4/19/99 52 05149911 Tox-120, RBL04199-500ppb-2,4/19/99 53 05149911 Tox-120, RBL04199-750ppb-2,4/19/99 54 05149911 Tox-120, RBL04199-1000ppb-2,4/19/99 TELMER 9min- 96 10 Analyte TELMER 9min- 96 10 Analyte TELMER 9min- 41 10 Analyte TELMER 9min- 42 10 Analyte TELMER 9min- 43 10 Standard 4.93 TELMER 9min- 44 10 Standard 9.76 ' TELMER 9min- 45 10 Standard 24.8 TELMER 9min- 46 10 Standard 49.3 TELMER 9min- 47 10 Standard 97.6 TELMER 9min- 48 10 Standard 248 TELMER 9min- 49 10 Standard 493 TELMER 9min- 50 10 Standard 735 TELMER 9min- 51 10 Standard 976 TELMER 9min- 96 10 Analyte TELMER 9min- 52 10 Analyte TELMER 9min- 53 10 Analyte TELMER 9min- 54 10 Analyte TELMER 9min- 55 10 Analyte TELMER 9min- 56 10 Analyte TELMER 9min- 96 . 10 Analyte TELMER 9min- 57 10 Analyte TELMER 9min- 58 10 Analyte TELMER 9min- 59 10 Analyte TELMER 9min- 60 10 Analyte TELMER 9min- 61 10 Analyte TELMER 9min- 62 10 Analyte TELMER 9min- 63 10 Analyte TELMER 9min- 64 10 Analyte TELMER 9min- 65 10 Analyte TELMER 9min- 97 10 Analyte TELMER 9min- 66 10 Analyte TELMER 9min- 67 10 Analyte TELMER 9min- 68 10 Analyte TELMER 9min- 69 10 Analyte TELMER 9min- 70 10 Analyte TELMER 9min- 97 10 Analyte TELMER 9min- 71 10 Analyte TELMER 9min- 72 ' 10 Analyte TELMER 9min- 73 10 Analyte TELMER 9min- 74 10 Analyte TELMER 9min- 75 x 10 Analyte TELMER 9min- 76 10 Analyte TELMER 9min- 98 10 Analyte TELMER 9min- 41 10 Analyte TELMER 9min- 42 10 Analyte TELMER 9min- 43 10 Standard 4.93 TELMER 9min- 44 10 Standard 9.76 TELMER 9min- 45 10 Standard 24.8 TELMER 9min- 46 10 Standard 49.3 TELMER 9min- 47 10 Standard 97.6 TELMER 9min- 48 10 Standard 248 TELMER 9mln- 49 10 Standard 493 TELMER 9min- 50 TELMER 9min- 51 10 Standard 735 10 Standard 976 ' Factor 1 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 000659 Scanning Mathod Report Method: C: \HXS8LniX\FACT-l. PR0UCQODS\TSXJaai9 Last Modified: frl M ay 14 15:30 01 1999 Printed: frl May 14 18:17x28 1999 olrent Daisy ( alas ) i 0.00 Function s 1 MUM of 3 Maas fairs ( U > - ) Inter Chaaasl Daisy ( Sacs J i Spaa ( Daltons ) : Start Tina ( Kins ) : Bad Tina ( Kins ) : Repeat i Channel Parent Daughter 0.03 0.00 0.00 9.00 1 (Sacs) Coll B nergy (aV) Cona ( V ) HH 1 1 413.00 119.00 0.2S 2 413.00 169.00 0.25 3 413.00 219.00 0.25 30 20 30 15 IS 15 Function s 2 M M of 1* Mass Pair ( - ) . Inter Channel Delay ( Secs } t Spaa ( Daltons ) i Start Tina ( Mins ) i Snd Tina ( Mins ) i Repasts t Channel Parent Daughter 0.03 0.00 0.00 9.00 1 Dwell (Sm s ) Coll Bnergy (aV) Cone ( V ) 1 463.00 219.00 0.40 20 35 nineties : 2 MRK of 1 Mass Pair ( > Inter Channel Delay ( Secs ) : Span ( Daltons ) t Start Tina ( Kins ) i Bad Tine ( Kins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 9.00 1 Dwell (Sacs) Coll Bnergy (aV) Cone ( V ) 1 513.00 219.00 0.40 20 35 Function x 4 KKK of 1 Mass Pair ( BSP- ) Inter Channel Delay ( Secs ) : Span ( Daltons ) i Start Tina ( Mins ) i End Tine ( Mins ) : Repeats t Channel Parent Daughter 0.03 0.00 0.00 9.00 1 Dwell (Sacs) Coll Bnergy (aV) Cone ( V ) 1 563.00 219.00 0.40 25 30 Function s S HUM of 1 Mass Fair ( BSP- ) Inter Channel Delay ( Secs ) i Span ( Daltons ) i Start Tine ( Mins ) i Xnd Tine ( Mins ) i Repeats i Channel Parent Daughter 0.03 0.00 0.00 9.00 1 Dwell (Sacs) Coll Bnergy (aV) Cone ( V ) 1 13.00 219.00 0.40 20 40 function t * mat of 1 Mans falx ( BSP- ) Inter Channel Delay ( Sees ) : Span ( Daltons ) : Start Tine ( Kins ) : Snd Tine ( Mias ) i Repeats : Channel Parent Daughter 0.03 0.00 0.00 9.00 1 Dwell (Sacs) Coll Bnergy (aV) Cone ( V ) 1 427.00 80.00 0.40 40 60 Vl0* 1 000660 FACT: DATA REVIEW SUMMARY FORM Date: fls//e/Ti Analyst: FACT Study Number I Matrix Time Points Dilutions? Analyte 1: ' & + Z 3 ... |:35~J|'Jl/h). PoA A Acceptable LinearRange: , LOQ fix this data set / > Re-evaluated fix diffisent range? . Analyte 4: yl/1 S & 3 Acceptable Linear Range: --A ) 0 S T A jO- -- LOQ for this data set: * Re-evaluated for different range? -- . AnafyteS: />?,/3 AcceptableLipearRange: LOQ for this data set Re-evaluated for differentrange? Analyte 2: Acceptable T.inearRange: -- LOQ for this data set __________ ' Re-evaluated far different range? Analyte 3: TW AcceptableT.incarRange: LOQ for this data set / P j t f c -------------- Re-evaluated for different range? ^ fo r /W V & 3 Lw I (k .'fC ' A - b & y * - ( H V l. * 4 ^ 3 ^ A1563 JkiuUxis't* W f -V k , leA*H--hrv^JL fro - + U - d -b d v ^ - ftsVis/ft / " * / . v a . c w fe S '"4 /) / 'Jo D /;3S "d-0/M O 000661 cfe Q u a n tify Com pound Sum mary R a p o rt TOX-120 R a t L lv a r D ilu tio n Saltila U a t : S:\rACT-l.FRO\SaaplaDB\OS1499a Last modifind: Mon May 17 14:14:20 1999 M a t h od: S:\rxCS-l.FMO\MathDB\051499e Laat modlfiad: Mon May 17 14:23:38 1999 Job Coda: Frintad: Tua May II 09:22:40 1999 Compound 1: PCAX Maaa 1 051499081 2 051499082 3 051499083 4 051499064 5 051499065 6 051499066 7 051499067 S 051499068 9 051499069 10 051499070 11 051499071 12 051499072 13 051499073 14 051499074 15 051499075 16 051499076 17 051499077 18 051499078 19 051499079 20 051499080 21 051499081 22 051499082 23 051499083 24 051499084 25 051499085 26 051499086 27 051499087 26 051499088 29 051499089 30 051499090 31 051499091 32 051499092 33 051499093 34 051499094 35 051499095 36 051499096 37 051499097 38 051499098 39 051499099 40 051499100 41 051499101 42 051499102 43 0S1499103 44 051499104 45 051499105 46 051499106 47 051499107 48 051499108 49 051499109 SO 051499110 51 051499111 52 051499112 53 051499113 54 051499114 Sairplaliat Taxt MaOH Blank MOH Blank Tox-120, RBL04199-B20Blk-2, 4/19/99 Tox-120, *Bl04199-tSlk-2, 4/19/99 Tox-120, *BL04199-Sppb-2, 4/19/99 Tox-120, RBL04199-10ppb-2, 4/19/99 Tox-120, RBL04199-2Sppb-2, 4/19/99 Tox-120, BBL04199-50ppb-2, 4/19/99 Tox-120, BBD04199--100ppb-2, 4/19/99 TOX-120, NU.04199-250ppb-2, 4/19/99 Tox-120, *Bl04199-S00ppb-2, 4/19/99 Tox-120, BBL04199-750ppb-2, 4/19/99 Tox-120, XBL04199-1000ppb-2, 4/19/99 MaOH Blank Tox-120 23M 62 / D1-.2S Tox-120 24M G2 / Dl:25 Tox-120 25M G2 / Dl:25 Tox-120 23M G2 / DI:25 Tox-120, RBI.03199-- 2S0ppb-CCl, 4/19/99 H e O S Bl'ank Tox-120 33M G3 / Cl:25 Tox-120 34M G3 / Dl:25 Tox-120 35M G3 / Dl:25 Tox-120 36M G3 / DI:25 Tox-120 37M G3 / Dl:25 Tox-120 36M G3 / DI:25 Tox-120 39M G3 / DI:25 Tox-120 4OH G3 / DI:25 Tox-120, ABL04199--250ppb-CC3, 4/19/99 HaQH Blank /Tox-120 27M G2 /Tox-120 29M G2 /Tox-120 SOM G2 /Tox-120 31M G2 DI: 10 DI: 10 Dl:10 D i : 10 Tox-120, XBX*04199-250ppb-CC4, 4/19/99 KaOH Blank /Tox-120 42M G3 /Tox-120 4SM G3 /Tox-120 45M G3 /Tox-120 4 SM G3 /Tox-120 47M G3 DI: 10 DI: 10 DI: 10 DI: 10 DI: 10 Tox-120, RBL4199-250ppb-CC5, 4/19/99 M.OB Blank Tox-120, RBL04199-H2OBlk-2, 4/19/99 Tox-120, RBL04199-LBlk-2, 4/19/99 Tox-120, BBZi04199-5ppb-2, 4/19/99 Tox-120, BBL04199-- 10ppb-2, 4/19/99 Tox-120, RBL04199-25ppb-2, 4/19/99 Tox-120,- RBL04199-- 50ppb-2, 4/19/99 Tox-120, KBI*04199-100ppb-2, 4/19/99 Tox-120, RBL04199-230ppb-2, 4/19/99 Tox-120, RBl*04199-500ppb-2, 4/19/99 Tox-120, ABL04199-750ppb-2, 4/19/99 Tox-120, RBD04199-1000ppb-2, 4/19/99 Typ Analyta Analyta Analyta Analyta Standard Standard Standard Standard Standard Standard Standard Standard Standard Analyta Analyta Analyta Analyta Analyta OC Analyta Analyta Analyta Analyta Analyta Analyta Analyta Analyta Analyta OC Analyta Analyta Analyta Analyta Analyta OC Analyta Analyta Analyta Analyta Analyta Analyta OC Analyta Analyta Analyta Standard Standard Standard Standard Standard Standard Standard Standard Standard Std Cono 5.56 11.10 27.80 55.60 111.00 278.00 * 556.00 833.00 1121.00 278.00 278.00 278.00 278.00 5.56 11.10 27.80 55.60 111.00 278.00 556.00 833.00 1111.00 XT 3.050 3.047 3.030 3.049 5.049 5.033 3.043 5.048 5.050 5.048 5.049 5.049 5.049 5.048 5.050 5.050 3.050 5.053 5.049 3.048 5.049 5.049 5.050 5.048 5.049 5.050 5.050 5.048 5.049 5.048 5.049 5.048 5.049 5.052 5.048 5.049 5.051 5.050 5.049 5.050 5.050 5.049 5.048 5.051 Paga 1 Asta Xtsponn Cena. Flag IDc t 72 132 113 175 406 801 1123 1283 368 592 283 255 466 383 601 481 . 515 503 591 465 598 485 440 268 281 326 508 263 563 214 177 288 471 81 58 113 39 139 105 249 429 837 1175 1380 71.666 132.374 113.329 175.242 406.110 800.930 1122.779 1282.724 368.371 592.299 282.603 254.927 463.685 382.606 601.330 480.556 515.341 502.581 590.622 464.784 597.567 485.149 439.886 268.097 280.775 325.677 508.135 262.546 562.997 213.511 177.013 287.691 471.073 81.083 57.712 112.987 38.519 138.857 104.892 248.672 429.161 837.128 1175.497 1379.791 9.88 Mf 78 53.49 bb 41.18 bb 87.71 bb 231.22 bb 557.95 bb 799.83 bb 920.04 bbX 100 -26 -21 -6 0 -4 -17 232.86 bb 401.15 bb 168.40 bb 147.60 bb 304.49 bb \\ 10 243.55 bb 407.94 bb 317.17 bb 343.31 bb 333.72 bb 399.89 bb 305.32 bb 405.11 bb 320.62 bb 266.60 bb 157.50 bb 167.02 bb 200.77 bb 337.90 bb // \1S ( 22 153.32 bb 379.13 bb 116.47 bb 89.04 bb 172.22 MK 310.04 bb 12j'/j 16.95 KH 0.00 MH 40.92 fabX 636 0.00 MK -100 60.37 bb 117 -i34.84 bb -37 142.90 bb . 29 278.54 bb 0 585.15 bb 5 839.45 bb 1 992.99 MMX -11 BESTCOPYAVAILABLE S o u p 0 2 0 1 9 9 , K o v lo v o d odi q u a n t i t a t a r i toy d r b 5 / 1 7 / 9 9 000662 TOX-120 Rat U v a s Dilution 1080 1367 1207 1023 MHZ bbl MMI MHZ MHZ Soup 020199, R f t v i m d and quantltatad by drb 5/17/99 & & H MH H 3222 S X mXXXXX HHHH 2222 Is r pk s I . Ss s SSssp iiii 3SsS ssc ssa ss S2aS m S isa s 8SS53 32223 S3SS S3S535SS I l i a S5SSS sasssssss 3 "388=5353 3 s s s5 s sassgggg i S B gjgg 31111*3 5 5 . . i P P P i P * * * * m m m m u min n m u m ih in /t n i ln a n Uljn i HtHrmH Hh PP * g* e 22 -1 s a Mi n ils assaf aaaaaaaaf saass aaaaa SaSaSaSjj; NaNsWNSaNaNidg SaSaNaaS? aaaaa I S888S 833388383 88883 38833 .saaaaaaaass^a^asggisa^sgsa^sssg^asaaagssass^ *3^s<SSaS^S^^SSS^^ m m m nm m m m m m m m m m m m um iiliiilliliiiliiiliiililiilliilillilllliilliliiiiiilii JsSSSoSSo33S8oSoooSo88S2SS8SSSooooSSoSoSSoo383S3SSoSsio "-""-"''-''aaaasaaasaaaaaaaaRaaaasssssRsassiisssscsssaBSs CO W o o 1 Quantify Canpound S w a r y Raport TOX-120 Rat Livar Dilution Paga 3 1 Mano 1 051499061 2 051499062 3 051499063 4 051499064 5 051499065 6 051499066 7 051499067 S 051499068 9 051499069 10 051499070 11 051499071 12 051499072 13 051499073 14 051499074 15 051499075 14 051499076 17 051499077 18 051499078 19 051499079 20 051499080 21 051499091 22 051499082 23 051499083 24 051499084 25 051499085 26 051499086 27 051499087 28 051499088 29 051499089 30 051499090 31 051499091 32 051499092 33 051499093 34 051499094 35 051499095 36 051499096 37 051499097 38 051499098 39 051499099 40 OS1499100 41 051499101 42 051499102 43 051499103 44 051499104 45 051499105 46 051499106 47 051499107 4B 051499108 49 051499109 50 051499110 51 051499111 52 051499112 53 051499113 54 051499114 8aspilit Taxt HaOH Blank HaOH Blank Tox-120, RBL04199-H20BIk-2, 4/13/99 TOX-120, RBW)4199-lBlk-2, 4/19/99 Tox-120, RBL04199-5ppb-2, 4/19/99 Tox-120, BBl*04199-10ppb-2, 4/19/99 Tox-120, KBL04199-25ppb-2, 4/19/99 Tox-120, BBL04199-S0ppb-2, 4/19/99 Tox-120, X8L04199-100ppb-2, 4/19/99 Tox-120, RBL04199-2S0ppb-2, 4/19/99 Tox-120, 9BL04199-500ppb-2, 4/19/9.9 Tox-120, BBX04199-750ppb-2, 4/19/99 TOX-120, RBX041S9-10Q0ppto-2, 4/19/99 HaOH Blank TOX-120 23M 62 / 91:25 Tox-120 24M G2 / DI:25 Tox-120 2SH G2 / DI:25 Tox-120 2 62 / 91:23 Tox-120, RBL04199-250ppb-CCl, 4/19/99 HaOH Blank Tox-120 33H 63 / 91:25 Tox-120 34M 63 / 91:25 Tox-120 3SM 63 / 91:25 Tox-120 36M 63 / 91:25 TOX-120 3TH 63 / 91:25 Tox-120 3SM 63 / 91:25 Tox-120 39M 63 / 91:25 Tox-120 40N 63 / 91:25 Tox-120, BBL04199-250ppb-CC3, 4/19/99 MaOH Blank Tox-120 27H 62 / 91:10 Tox-120 29H 62 / 91:10 Tox-120 30M 62 / 91:10 Tox-120 31M 62 / 91:10 Tox-120, BBI>04199-250ppb-CC4, 4/19/99 HaOH Blank Tox-120 42H 63 / 91:10 Tox-120 43M 63 / 91:10 Tox-120 45M 63 / 91:10 Tox-120 4SM 63 / 91:10 Tox-120 47H 63 / 91:10 Tox-120, RBL04199-250ppb-CC5, 4/19/99 HaOH Blank Tox-120, RBL04199-H20Blk-2, 4/19/99 Tox-120, RBL04199--Ilk-2, 4/19/99 Tox-120, RBL04199-- 5ppb-2, 4/19/99 Tox-120, RBL04199-10ppb-2, 4/19/99 Tox-120, RBL04199-25ppb-2, 4/19/99 Tox-120.- BBL04199-50ppb-2, 4/19/99 Tox-120, BBL04199-100ppb-2, 4/19/99 Tox-120, ABL04199-250ppb-2, 4/19/99 Tox-120, BBL04199-500ppb-2, 4/19/99 TOX-120, RBL04199-750ppb-2, 4/19/99 Tox-120, BBL04199-1000ppb-2, 4/19/99 Typ Analyta Analyta Analyta Analyta Standard Standard Standard Standard Standard Standard Standard Standard Standard Analyta Analyta Analyta Analyta Analyta OC Analyta Analyta Analyta Analyta Analyta Analyta Analyta Analyta Analyta OC Analyta Analyta Analyta Analyta Analyta QC Analyta Analyta Analyta Analyta Analyta Analyta QC Analyta Analyta Analyta Standard Standard Standard Standard Standard Standard Standard Standard Standard ltd Cono Kt 5.56 11.10 27.80 55.60 111.00 278.00 ' 556.00 833.00 1111.00 5.466 5.463 5.464 5.464 5.465 5.500 5.464 5.514 278.00 5.515 ' 5.513 5.514 5.514 5.515 278.00 5.514 5.515 5.516 5.516 5.523 5.515 5.514 5.515 5.514 278.00 5.514 5.514 5.514 5.515 5.515 278.00 5.514 5.515 5.512 5.514 5.514 5.515 5.56 11.10 27.80 55.60 111.00 278.00 556.00 833.00 1111.00 5.516 5.515 5.513 5.514 5.516 5.515 5.513 5.516 iru RftSpOM* Cono. Flags %Dv 13 34 49 128 253 467 763 764 79 103 59 86 245 90 76 66 69 71 49 . 66 64 241 136 173 116 138 275 111 121 68 93 71 244 13.419 34.422 .48.961 127.672 253.440 466.900 763.341 764.046 10.23 MK 33.18 MK 49.07 MK 135.10 bb 272.54 bb 505.83 bb 829.80 bb 830.57 bbX 78.528 103.445 58.790 86.441 244.847 81.39 MK 108.62 bb 59.82 MK 90.03 bb 263.15 bb 89.556 93.44 bb 76.379 79.04 MK 65.982 67.68 MK 69.198 . 71.19 MK 70.905 73.06 MK 48.849 48.95 MK 66.234 67.95 MK 64.294 65.83 MK 241.294 259.27 bb 135.719 173.108 116.489 137.808 274.745 143.89 bb 184.75 bb 122.87 bb 146.17 bb 29S.83 bb 110.694 121.136 67.748 93.064 71.230 244.465 116.54 bb 127.95 bb 69.61 MM 97.27 bb 73.41 MK 262.74 bb 8 19 -12 22 -2 -9 0 -25 \ -5 -7 6 -5 15 14.743 11.68 MK 5 23 23.309 21.04 MK -24 50 50.399 50.65 MK * -9 116 116.114 122.46 b b . io 262 262.095 282.00 bb 1 547 546.872 593.23 bb 7 762 761.863 828.19 bb -1 773 772.968 840.32 MMX -24 i 1k l j f i j' S o u p 0 2 0 1 9 9 , R o v io w o d a n d q u a n t i t a t a d toy d r b 5 / 1 7 /9 9 000664 Quantify Ccxnpound Sunnary ltapert TOX-120 Rat U n r DUutiona 45.418 70.127 44.525 47.121 Soup 020199, Sviawd and quantitatad hy drb 5/17/99 SU NA CO ! a i i t sii . Ssi 558 523 ssis 3835 fi SSSSggggg SEE in ! " 5583S553 5 EBBE g8 55 g SSSSggggg 5 " ^ S r'SSH i ni m i i n u m i i m i m i n i l . I ssssi sssss 5 s s a s s s s s * aaaai a a a a a a I 55355555555 88885 888888885 83883 888883 5555555552 m0 H 1 ^SSSSSSSS^SS^SSSSS^SSSSSSSSS^SSSSS^SSSSaS^SSSSSSS'SSSS I iiiiiiiiiiiilliliiiliilifiiiiiiillliiliiiliil 1 lilffl3 H 3 3 m iltii H m m m iH n S U S n im m 2 "SSSSSnSSSSSSSSSSSRSSSriSRSSSSiSgSSSSSSgSgSSSKSS 1/3 <3 00 O O O am rm^ fiHi niitiomi m & 3 m aaa a g XPSPSSS s I KKSPSSS i s ! 555555 i ! 8853 S *2 NNrntiArtnHinlfrl|OH Nw s int5n 5 tn 5 5m5 w ' 3 " o1 x s s s s s s g g 3 "28323 S '5 1fH 0 iH aa O5 o r-8 Nr* 3 1n0 r ? o Hr t 2 Hn toft IfOi S13t 7 - 3 7 S1 2 ssisssl min 2S SS S SS frnit 2 3 3 S 5 N*C m m mfiH< 5 3 5 3 Mn 0HWfiiNArn<srn|mH 0i MS> tn 5in oo s mr- 5 Mem S S S 2 S S 3 tft inin ininwiin *oo S 5S S S S S S S ran* " * 2 5 3 2 3 555.. Siili I l i1 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 . i*iiiiiiiiiiiiiiiiiiiiiii il mi iiiiti55551 555.555.55s 55.5.51 8 **NNN7 3 3 8 8 ? 8 3 8 3 3 3 8 3 ? 3 3 3 3 ? 8 3 8 3 3 3MiO*-*r4nMoiior`f^ sN* N* v * 0 S S S X S f l S 83883838888 88833 383338888 88888 88833 8 S i l l l l 3 I I 3 l a 1 s s ! s 3 S 5 a 5 S | S | s 1 s * s a 5 a s a 5 f l 5 8 l a * s . a , jM 8 S $ $ S $ $ '3 S S S ! 3 S 3 S 5 S 3 8 S s S 5 5 3 a 3333333'aS '5'5'$$S S W lllllee83383s8l38 iililiiiliiiiliiiiiilliliiiiiiiilliiiiiilfiliiliililii Jssssssssssssssssssssssssssssosssssssssssssssssssssssss CO CO CO o o Soup 020199 Roviowod and quantitatod by drb 5/17/99 Q u a n tif y Ccs p o u n d Suinit r y R t p o r t TOX-120 S a t L i v a r D i l u ti o n s Sample List: S:\IACT-1.FR0\8a^leDB\O51499o Last modified: Mon May 17 14:14:20 1909 Method: S:\ISCT-l.PR0\Math0B\051499o Last modified: Mon May 17 14:22:39 1999 Job Coda: Printed: Tua May 1> 08:22:40 1999 Compound (: IS # Mima 1 051499061 2 051499062 3 051499063 4 051499064 5 051499065 051499066 7 051499067 0 051499068 9 051499069 10 051499070 11 051499071 12 051499072 13 051499073 14 051499074 15 051499075 16 051499076 17 051499077 18 051499078 19 051499079 20 051499080 21 051499081 22 051499082 23 051499083 24 051499084 25 051499085 26 051499086 27 051499087 28 051499088 29 051499089 30 051499090 31 051499091 32 051499092 33 051499093 34 051499094 35 051499095 36 051499096 37 051499097 38 051499098 39 051499099 40 051499100 41 051499101 42 051499102 43 051499103 44 051499104 45 051499105 46 051499106 47 051499107 48 051499108 49 051499109 50 051499110 51 051499111 52 051499112 53 051499113 54 051499114 SanvXaXi.t l u t M.0H Blank MaOH Blank Tox-120, RBL04199-H20Blk-2f 4/19/99 Tox-120, M104199-LBlk-2, 4/19/99 Tox-120, RBL04199-Sppb-2, 4/19/99 Tox-120, BBL04199-10ppb-2, 4/19/99 Tox-120, RBL04199-2Sppb-2, 4/19/99 Tox-120, RBL04199-50ppb-2, 4/19/99 Tox-120, BBL04199-100ppb-2, 4/19/99 TOX-120, BBL04199-250ppb-2, 4/19/99 Tox-120, RBL04199-500ppb-2, 4/19/99 Tox-120, 8BLQ4199--750ppb-2, 4/19/99 Tox-120, BBL04199-1000ppb-2, 4/19/99 MaOB Blank Tox-120 23K 62 / Dl:25 Tox-120 24K 62 / Dl:25 Tox-120 234 62 / 01:25 Tox-120 26M 62 / Dl:25 Tox-120, RBL04199--250ppl>-CCl, 4/19/99 HeOH Blank Tox-120 33M 63 / D1:2S Tox-120 34M 63 / 01:23 Tox-120 334 63 / 01:25 Tox-120 304 63 / 01:25 Tox-120 37M 63 / 01:25 Tox-120 3BM 63 / 01:25 Tox-120 39M 63 / 01:25 Tox-120 40M 63 / 01:25 Tox-120, RBL04199-250ppb-CC3, 4/19/99 MeOH Blank Tox-120 27K 62 / 01:10' Tox-120 29K 62 / 01:10 Tox-120 SOM 62 / Dl:10 Tox-120 31M 62 / 01:10 Tox-120, RBL04199-2S0ppb-CC4, 4/19/99 MaOH Blank Tox-120 42M 63 / Dl:10 Tox-120 43M 63 / Dl:10 Tox-120 45M 63 / 01:10 Tox-120 44M 63 / 01:10 Tox-120 47M 63 / 01:10 Tox-120, RBL04199-250ppfa-CC5, 4/19/99 MaOH Blank Tox-120, BBL04199-H20Blk-2, 4/19/99 Tox-120, BBL04199-lBlk-2, 4/19/99 Tox-120, 9BL04199--Sppb-- 2, 4/19/99 Tox-120, BBL04199-10ppb-2, 4/19/99 Tox-120, BBL04199-25ppb-2, 4/19/99 Tox-120, RB104199--50ppb-2, 4/19/99 Tox-120, RB1.04199--lOOppb-2, 4/19/99 Tox-120, BBL04199--250ppb-2, 4/19/99 Tox-120, BBl04199-500ppb-2, 4/19/99 Tox-120, RBL04199-750ppb-2, 4/19/99 Tox-120, KB104199-1000ppb-2, 4/19/99 Typ Analyta Analyta Analyta Analyta Standard Standard Standard Standard ' Standard Standard Standard Standard Standard Analyta Analyta Analyta Analyta Analyta QC Analyta Analyta Analyta Analyta Analyta Analyta Analyta Analyta Analyta QC Analyta Analyta Analyta Analyta Analyta QC Analyta Analyta Analyta Analyte Analyta Analyte QC Analyta Analyta Analyta Standard Standard Standard Standard Standard Standard Standard Standard Standard Std Cono St 1.00 1.00 1 a 00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 5.036 5.035 5.036 5.036 5.033 5.036 5.034 5.035 5.023 5.034 5.034 5.036 5.034 ' 5.035 5.035 5.035 5.034 3.036 5.036 5.036 5.042 5.035 5.034 5.035 5.035 5.037 5.034 5.035 5.036 5.036 5.034 5.035 5.034 5.035 5.034 5.035 5.038 5.034 5.035 5.037 5.036 5.035 5.036 5.036 5.035 5.034 5.037 Area 2407 2496 2699 2722 2446 2280 2566 2352 2408 2309 2302 81 109 74 70 2336 170 81 71 95 84 83 . 97 73 2253 163 198 184 179 2464 214 175 164 no 161 2414 2416 2396 2542 2751 2SOO 2337 2586 2464 2333 2355 2457 Reponce Cene. Slags %Dev 2406.723 2496.454 2699.373 2722.382 2446.267 2280.384 2565.513 2351.564 2408.171 2308.686 2301.694 81.237 109.041 74.247 69.750 2336.227 169.517 80.550 71.387 94.601 84.019 82.882 96.582 72.744 2253.416 163.472 198.362 183.888 178.796 2464.372 213.740 174.571 163.908 169.648 160.737 2413.697 2415.683 2395.952 2541.736 2751.209 2500.397' 2336.569 2585.568 2463.607 2333.406 2355.073 2457.479 0.98 bb 1.01 bb 1.09 bb 1.10 bb 0.99 bb 0.92 bb 1.04 bb 0.95 bb 0.98 bb 0.94 bb 0.93 bb -2 1 9 10 -1 -8 4 -5 -2 -6 -7 0.03 bb 0.04 bb 0.03 m 0.03 MM 0.95 bb -97 -96 -97 -97 -5 0.07 bb 0.03 bb 0.03 MM 0.04 bb 0.03 bb 0.03 bb 0.04 bb 0.03 MM 0.91 bb -93 -97 -97 -96 -97 -97 -96 -97 -9 0.07 bb 0.08 bb 0.07 bb 0.07 bb 1.00 bb -93 -92 -93 -93 0 0.09 bb 0.07 bb 0.07 bb 0.07 bb 0.07 bb 0.98 bb -91 -93 -93 -93 -93 -2 0.98 bb 0.97 bb 1.03 bb 1.12 bb 1.01 bb 0.95 bb * 1.05 bb 1.00 bb : 0.95 bb 0.95 bb 1.00 MM -2 -3 3 12 1 -5 5 0 -5 -5 0 Paga 6 Soup 020199, S a v ia wad an d q u a n tita te d b y d sb 5 /1 7 /9 9 000667 Q u an tify C a lib ra tio n S a p o rt Tax-120 a t l i v a r D i l u t i o n s Calibration s B:\raCT-l.PRO\CurvarB\05UaJa Last aedifiad: Tua May 1 01:21:03 1999 Printad: Tua May 18 00:22:33 1909 Paga 1 * Ooup 020199, K aviavad and q u a n tita ta d b y dxb 3 /1 7 /9 9 000668 Q u an tify C a lib ra tio n R ap o rt TCX-120 b a t Zalvor O l l u tl o n a Calibration: i:\rACT-l. rao\CurvDB\051499o Laat aodlflad: Tun May 18 08:21:03 1999 Prlntad: Tua Kay 18 08:22:83 189 Paga 2 000669 Q u an tify C a lib ra tio n P a p o rt T0K -120 P a t L lv a r B llu tlo n a C a lib r a tio n s S :\yP C T -l.P 9O \C urvaD B \0S 1499a l a a t n o d l f i a d i T ua May 1* 0 3 :3 1 :0 3 1339 P rln ta d : T ua May 13 0 3 :2 3 :3 3 1999 Pago 3 Q u a n tify C a lib ra tio n R ap o rt TOX-120 R a t U v a r D llu tio n a Calibration: I:\Plcr-l.PRO\CurMD8\051499o Laat nodlflad: Tun May It 08:21:03 1989 trlntad: tun Kay 19 08:22:53 1999 Paga 4 Soup 0 2 0 1 9 9 , R arvlaw ad a n d q u a n t i t a t a d b y d r b 5 /1 7 /9 9 000671 Q u an tify C a lib ra tio n K aport TGX-120 M at L lv a r O il u tlo n a C a l i b r a t i o n 8 :\F A C T -1 .PR O \C urvoD B \Q 51498c L a s t a o d if l a d : Tua M ay 18 0 8 :2 1 1 0 3 1888 P rin ta d : Tua May 18 0 8 :2 3 :3 3 1888 faga 5 Soup 020188, Raviawad and quanti tatad by drb S/17/88 000672 1 Q u a n t i f y Ca l i b r a t i o n B a p o r t (ax-120 B a t U v a r D l l a t l a n a lalibration! S:\XBCT-l.Pie\eanrtfB\0S14BBa 1 U a t aodiflad: Tua May IB 08:21:03 1898 (rintad: Tua May IB 08:22:53 1999 Compound 6 name: IS 1 Response Factor. 2467.17 Response type: External Std, Area Curve type: RF I 1 3 I 1 1 ! ; i I I J 1 3 ! J ;i ? Paga Method Report Method file: Last modified: Compound: Printed: S:\IACT-l.PBO\MethDB\051499c.mdb Mon Hay 17 14:23:3 19990 1: PQAA Tue Hey 18 09:41:43 1999 Compound Name: Zntemel Ref.: Quantify Trace: Cone, of Standards: User fUT Value: User Peak rector: Integrate Window rector: Peak location Retention Time (mins) : Relative Retention* Time: Time Window (mins) : Peak Selection: Response Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: rit 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: POAA [None] TZC Cone. A 1.000000, Disabled 1.000000 2 .0 0 0 4.998, Enabled 0.000, Disabled 0.400 Nearest External Areas Linear Exclude 1/X None 140 Disabled 3 2 20.00 100.00 0.00 10.00 Disabled 40.00 1.50, Disabled 0.00, Disabled 2.00, Disabled 90.00, Enabled Page l 000674 M athod R e p o rt Mathod fila: Last modified: Compound: P rin te d : 9:\FACT-l.PRO\MethDB\05I499c.mdb Mon May 1? 14:23:39 19990 2: M463 Tua May 18 0 9 :4 1 :4 3 1999 Conpound Hama: Internal Ref.: Quantify Traeai Cone, of Standards: Caer RT Valua: Oaar Peak ractor: Intgrata Hlndow factor: Peak Location Retention Time (mins): Relative Retention Time: Time Window (mins): Peak Selection: Response Response Type: Raeponse: Calibration Curves Polynomial Type: Point of Origin: Pit Weighting: Axis Transformation: Concentration Dnita: Noise Peak-to-pak anpiitndei Smooth Smoothing: Window size (scans): Number of smooths: Smoothing method: Bsselines Join valley threahold: Rduca peak tailing: Raiaa baseline naxlxun: Peak Seoaration Draw vertical threahold: Detect ahouldera: Shoulder threahold: Response Threshold Relative height: Rbaolute height: Relative area: Absolute area: M463 [None] TIC Cone* A 1.000000, Disabled 0.000000 2.000 5.40, Enabled 0.000, Disabled 0.551 Nearest external Areas Linear exclude 1/X Hone 140 Disabled 3 2 20.00 100.00 0.00 10.00 Disabled 40.00 1.50, Disabled 0.00, Disabled 2.00, Disabled 90.00, Enabled Sp/in 0 2 0 1 ^ -------------------------------------------- W c ojt/ W m .X Paga 2 000675 Hathod Report Method file: Last Modified: Compound: Printed: S:\PACT-l.PAO\MethBB\OS1499e.mdb Mon May 17 14:23:3 19990 3: MS13 Tue May 18 01:41:45 1999 Compound Hama: Internal Ref.: Quantify Trace: Cone, of Standards: Uses RF Value: D i m Peak Factors Integrate Window Factors Paak Location Retention Time (mine): Relative Retention Timet Tina Window (mins): Paak Selection: Response Raspons. Type: Response: Calibration Curves Polynomial Typos Point of Origin: Fit Weighting: Axis Transformation: Concentration Units: Holao Pealc-to-pealt aapiltude: Smooth Smoothing: Window size (scans): Humber of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: Paak Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative area: Absolute area: M513 (Hone) TIC Cone. A 1.000000, Disabled 1.000000 2 .0 0 0 5.538, Knablad 0.000, Diaablsd 0.325 Maaraat external Areas ' Linear Exclude 1/X None 140 Disabled 3 2 20.00* 100.00 0.00 10.00 Disabled 40.00 1.50, Disabled , 0.00, Disabled 2.00, Disabled 80.00, Enabled Sp(r*ya fr lP ill Page 3 000676 M ethod R e p o rt Method file: test Bodifled: Compound: P rin te d : S:\IACT-l.PRO\Nathna\0S1499c.ndb Mon Key 17 14:23:3 19990 4: M S 63 Tue Key 1 0 8 :4 1 :4 1999 Compound Nana: Internet Ref.: Quantify Trees: Cone, of Standards: User RF Vslusi Usar Peak Factors Integrate Window Factors Paak location Ratantion Time (Bins) : Relative Ratantion Tina: Tina Window (mins)s Paak Salactions Raaponaa Rasponsa Type: Rasponsas - Calibration Curves Polynomial Typas Point of Origins Fit Weighting: Axis Transformations Concantratlon Units: Koisa Peak-to-paak amplitude: Smooth Smoothings WlndoH size (seens): Mumbar of smooths t Smoothing methods Basallnas Join valley threshold: Reduce peek telling: Relse baseline Milieu: Peek Ssuaretlon Drew vertical threshold: D a t e d shoulderss Shoulder threshold: Response Threshold Rslstive height: Absolute height: Relative area: Absolute area: MSC3 (None] TIC Cone. A 1.000000, Dlaablad 1.000000 2 .0 0 0 5.349, Enabled 0.000, Dlaablad 0.51B nearest External Areas Linear Exclude 1/X Mona 140 Disabled 3 2 20.00 100.00 0.00 10.00 Dlaablad 40.00 1.50, Disabled < 0.00, Disabled 2.00, Disabled 10.00, enabled 'tH P n 0 liefr\ tx ito lfl Paga 4 | 000677 Method Report Method fllo: Loot modified: Com pound: P rin te d : S:\FACT-l.PR0\MethDB\0S1499c.mdb Mon Hoy XT 14:23:3 19990 5 : H613 Tue May 18 0 1 :4 1 :4 6 1999 Compound Nemo: Internal R e f .: Quantify Trace: Cone, of Standards: Deer RP Value: Dser Peak factor: Integrate Window factor: Peak location Retention Time (mins): Relative Retention Time: Time Window (mins): Peak Selection: Response Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: fit Weighting: Axis Transformation: Concentration Chits: Mol am Peak-to-pest amplitude: Smooth Smoothing: Window sis (scans): Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raisa baseline maximum: Peak Seoaration Draw vertical threshold: Detect shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative area: Absolute area: M613 [MOne] TIC Cone. A 1.000000, Disabled 1.000000 2 .0 0 0 5.S3, Enabled 0.000, Disabled 0.27S nearest External Areas lilnesr Exclude 1/X Hone ' 140 Disabled 3 2 20.00 100.00 0.00 10.00 Disabled 40.00 1.S0, Disabled , 0.00, Disabled 2.00, Disabled 0.00, Enabled Peg* S 000678 Method Report Method file: last Modified: Conpound: Printed: S:\lKT-l.PRO\MethDB\051499c.ndb Mon M ay 17 14:23:38 19990 6: is Tue May 18 08:41:48 1999 Conpound Nana: Internal Ref.: Quantify Trace: Cone, of Standards: Oser RT Value: Daer Peak Factor: Integrate Window Factor: IS [Done] TIC fixed 1.000000, Disabled 1.000000 2 .0 0 0 Peak Location Retention Tine Inins): Relative Retention Tine: Tine Window Inins): 5.034, Enabled 0.000, Disabled 0.200 Peak Selection: Nearest Rasoonsa Response Type: Response: external Areas Calibration Curves Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Linear Exclude 1 /X Hone Concentration Units: Holsa Peak-to-peak amplitude: 140 Smooth Smoothing: Window size (scans}: Humber of smooths: Smoothing method: Disabled 3 2 Baselines Join valley threshold: Reduce peak tailing: Raise baseline nsxiaun: 20.00 100.00 0.00 Peak Sesaratlon Draw vertical threshold: Detect shoulders: Shoulder threshold: 0 10.00 Disabled 40.00 Response Threshold Relative height: Absolute height: Relative area: Absolute area: 1.50, Disabled t 0.00, Disabled 2.00, Disabled *0.00,. Enabled b D L 1! M c, x /i /^9 rage 5 000679 SOUP 020199: FACT Equipm ent L og 99014 Q uattro II, #6414E DATE: 05/21/99 ANALYST: drb STUDY NUMBER: TQX-120 MATRIX:Rat Liver _DESCRIPTION: Pilutjons/Tclmer FACT Method: ETS-8-$Q ^ Injection volume: 10 uL Cycle time:.. ? TOIL Electrode:.Z-$pi ay----------- M obile Phase: fAtt.OmM NH4CH3CQ2 (B).MsOH--------------- :-- TN-A- or stndrd number (A) '99011-6-9_________ . (B )T-A-254S Prepared (date/by): Expires: (Al 04/28/99 drb_______ _ (A) 10/99---------------------- (B) 05/^1/99 a h fBl 10/99 Store at room temp? @ or N Other:. Guard column: None__________________ Part number: na_________ ' Lot number:jja-------------------------------- A nalytical colum n: Keystone Bctasil -------------------------------- _ _ _ _ _ Size: 2 x SO mm________________ Type: C l8____________ Sphere size:Jjm a---------- Part number: 055-701-2__________ Lot number: P7LQ4 Serial number:Q481175Z A nalytical parameters: Drying gas (IVhrl: 350 ESI nebulizing gas (L/hr)J5___ Sheath gas (L/hr)_0 LC Flow rate: 300 uL/min, Back pressure: 55 bar HPLC solvent gradient: 9min-2 Tinte (m in.l 110.00 211.00 3 1 4 ,5 0 4 1 6 .5 0 51 7.00 -%B 40,0 40.0_ _95.Q_ 95.0 40.0_ 000680 Tuning Method Report Method: C :\MASSLW0C\PACT-1 .PR0\ACQTOB\PF0S2 Printed: Fri May 21 16:28:16 1999 Rage 1 best copy available MS SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. MS2 Set Rdbk 3.01 40 5 0.2 150 250 3.01 -46 -8 153 254 Pressures Analyser Vacuum Gas Cell Rdbk 2.4e-4 4.8e-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier ."x MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set Rdbk 14.0 14.0 2.0 -Jl o.o ''* ' 53 650 Set Rdbk i5.0 15.0 45 43 2.0 0.0 40 39 0 43 650 000681 BESTCOPYAVAILABLE M aaslynx - Sam ple List Sample List: C:\MASSLYNX\FACT-1 .PRO\Sam pleDB\052199b.SPL Printed: Fri May 21 16:28:031999 Fite Nam e Fite T ext 1 052199068 MeOH Blank 2 052199069 MeOH Blank 3 052199070 Tox-120, R 8L04199-H 20B lk-1,4 /1 9 /9 9 4 052199071 Tox-120, RBL04199-LBIk-1,4/19/99 5 052199072 Tox-120, RBL04199-5ppb-1,4/19/99 6 052199073 Tox-120, RBL04199-1 Oppb-1,4/19/99 7 052199074 Tox-120, RBL04199-25ppb-1,4/19/99 8 052199075 Tox-120, RBL04199-50ppb-1,4 /1 9 /9 9 9 052199076 Tox-120, RBL04199-100ppb-1,4 /1 9 /9 9 10 052199077 Tox-120, RBL04199-250ppb-1,4 /1 9 /9 9 11 052199078 Tox-120, RBL04199-500ppb-1,4 /1 9 /9 9 12 052199079 Tox-120, RBL04199-750ppb-1,4 /1 9 /9 9 13 052199080 Tox-120, RBL04199-1000ppb-1,4 /1 9 /9 9 14 052199081 MeOH Blank 15 052199082 Tox-120 4 9 M G 4 /D 1 :1 0 16 052199083 Tox-120 5 0 M G 4 /D 1 :1 0 17 052199084 Tox-12051M G 4 /D 1 :1 0 18 052199085 Tox-120 5 2 M G 4 /D 1 :1 0 19 052199086 Tox-120, RBL04199-250ppb-CC1,4 /1 9 /9 9 20 052199087 MeOH Blank 21 052199088 Tox-120 5 3 M G 4 /D 1 :1 0 22 052199089 Tox-120 5 4 M G 4 /D 1 :1 0 23 052199090 Tox-120 5 5 M G 4 /D 1 :1 0 24 052199091 Tox-120 5 6 M G 4 /D 1 :1 0 25 052199092 Tox-120. R BL04199-250ppb-CC3,4/19/99 26 052199093 MeOH Blank 27 052199094 Tox-120 6 5 M G 5 /D 1 :5 0 0 28 052199095 Tox-120 6 6 M G 5 /D 1 :5 0 0 29 052199096 Tox-120 6 7 M G 5 /D 1 :5 0 0 30 052199097 Tox-120 6 8 M G 5 /D 1 :5 0 0 31 052199098 Tox-120, RBL04199-250ppb-CC11,4/19/99 32 052199099 MeOH Blank 33 052199100 Tox-120 69M G 5 /D 1 :5 0 0 34 052199101 Tox-120 70M G5 / 0 1 :500 35 052199102 Tox-120 71M G 5 /01:500 36 052199103 Tox-120 7 2 M G 5 /D 1 :5 0 0 37 052199104 Tox-120, RBL04199-250ppb-CC1,4 /1 9 /9 9 38 052199105 MeOH Blank 39 052199106 Tox-120 7 3 M G 5 /D 1 :2 5 0 40 052199107 Tox-120 7 4 M G 5 / D1:250 41 052199108 Tox-120 7 5 M G 5 /D 1 :2 5 0 42 052199109 Tox-120, R BL04199-250ppb-CC11,4/19/99 43 052199110 MeOH Blank 44 052199111 Tox-120 7 7 M G 5 /D 1 5 5 0 45 052199112 Tox-120 78M G5 / D1:250 46 052199113 Tox-120 79M G 5 /01:250 47 052199114 Tox-120, RBL04199-250ppb-CC1,4 /1 9 /9 9 48 052199115 M eO H Blank 49 052199116 Tox-120, R BL04199-H20Blk-1,4 /1 9 /9 9 50 052199117 Tox-120, R BL04199-LBIk-1,4/19/99 51 052199118 Tox-120, RBL04199-5ppb-1,4 /1 9 /9 9 52 052199119 Tox-120, RBL04199-1 Oppb-1,4/19/99 53 052199120 Tox-120, RBL04199-25ppb-1,4 /1 9 /9 9 54 052199121 Tox-120, RBL04199-50ppb-1,4/19/99 55 052199122 Tox-120, RBL04199-100ppb-1, 4/19/99 56 052199123 Tox-120, RBL04199-250ppb-1,4 /1 9 /9 9 57 052199124 Tox-120, RBL04199-5Q0ppb-1,4 /1 9 /9 9 58 052199125 Tox-120, RBL04199-750ppb-1, 4/19/99 59 052199126 Tox-120, RBLQ4199-1000ppb-1, 4/19/99 M S File TEU -PF2 TE -PF2 T E L I-P F 2 T E L I-P F 2 TEU -PF2 T E L I-P F 2 TEU -PF2 T E L I-P F 2 TEU -PF2 . TEU -PF2 T E L I-P F 2 TEU -PF2 TEU -PF2 TE -PF2 TEU -PF2 TEU -PF2 TEU -PF2 T E L I-P F 2 TE -PF2 T E -P F 2 TEU -PF2 TEU -PF2 TEU -PF2 TEU -PF2 T E -P F 2 T E U -P F 2 TEU -PF2 T E U -P F 2 TEU -PF2 T E L I-P F 2 T E L I-P F 2 T E L I-P F 2 TEU -PF2 T E U -P F 2 TEU -PF2 T E U -P F 2 TE -PF2 TEU -PF2 TEU -PF2 TEU -PF2 TEU -PF2 T E U -P F 2 TEU -PF2 T E U -P F 2 T E U -P F 2 T E U -P F 2 T E U -P F 2 TEU -PF2 TEU -PF2 TEU -PF2 T E U -P F 2 TEU -PF2 T E U -P F 2 T E U -P F 2 T E U -P F 2 T E U -P F 2 T E U -P F 2 T E L I-P F 2 T E U -P F 2 In let File B ottle ilum e 9m in-2 9m ln-2 9m in-2 9m in-2 9m ln-2 9m ln-2 9m In-2 9m ln-2 9m ln-2 9m in-2 9m in-2 9m In-2 9m ln-2 9m in-2 9m ln-2 9m in-2 9m ln-2 9m ln-2 9m in-2 9m in-2 9m ln-2 9m in-2 9m ln-2 9m in-2 9min-2 9m in-2 9mln-2 9m in-2 9m in-2 9mtn-2 9m ln-2 9m ln-2 9m in-2 9m in-2 9m ln-2 9m In-2 9m ln-2 9m in-2 9m in-2 9m in-2 9m ln-2 9m in-2 9m in-2 9m ln-2 9min-2 9min-2 9mln-2 9m in-2 9m in-2 9m In-2 9m in-2 9m in-2 9m in-2 9m in-2 9m ln-2 9m in-2 9m In-2 9m ln-2 9m ln-2 91 91 79 80 81 82 83 84 85 86 87 88 89 92 57 58 59 60 90 96 61 62 63 64 99 92 65 66 67 68 100 93 r 69 70 71 72 90 94 73 74 75 100 95 76 77 78 90 96 79 80 81 82 83 84 85 86 87 88 89 . 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 10 10 10 10 to 10 10 10 10 10 10 10 10 10 10 000682 Scanning1Method Report Method: C: \KU8tfna\FACT-l.TS0\JU5QOBS\TSLX-TF2 Last Modified: Tri Hay 21 15:13*53 1999 Triated: Tri May 21 16:20:25 1999 olvwt Mliy ( a i m I t 0.00 Function s 1 MM( of 2 Mesa M i n ( m - ) Xntar O u n l Dilay ( Sees ) : Span ( Dalton. > i Sturt Tima ( >lias ) i Sad Tina ( Mins ) i Kapaatf i Channel Taraat Daughter 0.03 0.00 0.00 9.00 1 Dwell (S.c.) Coll Energy (*V) Con. ( V ) 1 399.00 99.00 0.25 2 399.00 130.00 0 *2 5 45 45 60 60 Function i 2 MRM of 2 Mass Taira ( sar- > Zatar Channel Delay ( Sac. ) Spaa ( Daltoas ) t Start Tim. ( Mia. ) Sad Tine ( Mias ) : Repeats : Channel Taraat Daughter 0.03 0.00 0.00 9.00 1 Dwell (Seca) Coli B u r g y (V) . Con. C V ) 1 299.00 99.00 0.25 2 299.00 130.09 0.25 45 43 60 60 Juaetloa t 2 W M of 1 Mass Talr ( U T - ) Intar Channel Daisy ( Secs ) t 0.03 Spaa ( Daltons ) * Start Tina { Mias ) : 0.04 0.00 Sad Tina { Mias ) : 9.00 Repeats : 1 Channel parent Daughter Ovali (Sacs) Coll Knargy <aV) Cono ( V ) 1 427.00 80.00 0.23 40 00 **ge i 000683 FACT: DATA REVIEW SUMMARY FORM Date: S M H S _______ 000684 Tocnao-cs dilati a p i* U s ti cxm iiL nm rA C T -i.fK o\*^ia6a\03ais L u i a o d l t l t d * Mon Mty 24 0 0 i0 3 i0 9 1 H I M athedi e I\jttj* L Y \w u rr-i .9no\M atfcn\os3i99k U * t a a d i t l a i i Noa May 24 0 7 iS 9 i4 4 1991 t r i t li Iter 34 O ltlO iSS 1999 it m a Nmm 1 052199044 2 052199049 1 052199070 4 052199071 S 052199072 4 052199073 7 052199074 052199075 9 052199074 10 052199077 11 052199079 12 052199079 13 092199040 14 052199041 15 052199042 14 052199043 17 052199044 14 052199045 19 052199044 20 052199047 21 052199044 22 052199049 23 052199090 24 052199091 25 052199092 24 052199093 27 052199094 24 052199095 29 052199094 30 052199097 31 052199094 32 052199099 33 052199100 34 052199101 35 052199102 34 052199103 37 053199104 34 052199105 39 052199104 40 052199107 41 052199104 42 052199109 43 052199110 44 0S21991U 45 052199112 44 052199113 47 052199114 44 052199115 49 052199114 50 052199117 51 052199119 52 052199119 53 053199130 54 052199131 55 052199132 54 052199123 57 052199124 54 052199125 59 052199124 S tx p ltlla t tank MtOH S ita le MtOH S ita le Tox-120. M lL04139-K20Slk-l, 4/19/99 Tox-120, xaL04199-bBlfc-l. 4/19/99 TOX-120, HBL04199-Sppb-1, 4 /19/99 TOX-120, HBL04199-10ppb-l, 4 /1 9 /9 9 Tox-120, XSL04199-25ppb-l, 4/19/99 Tox-120, M L04199-50ppb-l, 4/19/99 T ox-120, ftBL04199-100ppfe~l, 4 /1 9 /9 9 Tox-120, M L04199-250ppb-l, 4/19/99 Tox-120, M U 4199-500tpb-l, 4/19/99 Tox-120. XBL04199-750ppb-l, 4/19/99 Tox-120, XBL0419t-1000ppb-l, 4/29/99 MoOH a ita la Tox-120 49M 04 / O l i 10 Tox-120 SOM 04 / 01*10 Tox-120 S1M 04 / O l i l O Tox-120 52M 04 / 01*10 Tox-120, UL04199-250ppb-CCl. 4/19/99 Mao a ita le Tox-120 S3M 04 / 0 1 :1 0 Tox-120 S4M 04 / O lilO TOX-120 S5K 04 / O lilO Tox-120 5 SM 04 / 01*10 Tox-120, ML04199-250ppb-CC3, 4/19/99 Mooa a ita le Tox-120 <5M OS / O l i 500 Tox-120 44M OS / O l i 500 Tox-120 47M OS / OliSOO TOX-120 4M OS / 01*500 Tox-120, M U 4199-2S tlprh CC11, 4/19/99 Htoa a ita li Tox-120 C9M 05 / 01*500 Tox-120 70M OS / 01*500 Tox-120 71M OS / 01*500 Tox-120 72M OS / 01*500 Tox-120, RBL04199-250ppb-CCl 4 /1 9 /9 9 MtOH a ita le Tox-120 73K OS / 01*250 Tox-120 74M OS / D lt2S0 Tox-120 7 SM OS / DI 250 TOX-120, M LO4190-25Oppb-CCll, 4/19/99 MtOH a ita le Tox-120 77M 05 / 01*250 Tox-120 7W Q 5 / 01*250 Tox-120 79M OS / 0 1 i2S0 Tox-120, XabO42JJ-250pffe-CCl, 4/29/99 MtOH a ita le Tox-120, JtaL04199-K2Oai)c-l, 4 /1 9 /9 9 Tox-120. K U 04199-LBlk-l, 4/19/99 Tox-120, RBL04199-Sppl>-1, 4 /1 9 /9 9 Tox-120, RSL04199-10ppb-l, 4/19/99 Tox-120, U L04199-29ppb-l, 4/19/99 Tox-120, 2BU)4199-S0ppb-1, 4/19/99 Tox-120, U L 04199-100ppb-l, 4/19/99 T ox-120, MBL04199-2S0ppb-l, 4 /1 9 /9 9 Tox-120, KBL04199-500ppb-l, 4/19/99 Tox-120, aaL04199-750ppb-l, 4/19/99 T ox-120, 2BC,04199-I000ppl>-1, 4 /1 9 /9 9 Typt A atly tt A atly tt A atly tt A atly tt S ta n d ard Standard S ttad trd Standard S ta n d ard Standard Standard Standard S e a n d trd A atly tt A atly tt A atly tt A atly tt A atly tt OC A atly tt A atly tt A atly tt A atly tt A atly tt oc A atly tt A atly tt A atly tt A atly tt A atly tt OC A atly tt A atly tt A atly tt A atly tt A atly tt OC A atly tt A atly tt A atly tt A atly tt oc A atly tt A atly tt A atly tt A atly tt OC A atly tt A atly tt A atly tt S ttad trd S ttad trd S ttad trd S ttad trd S ttad trd S ttad trd S ttad trd S ttad trd S ttadtrd s td eoa 5.54 11.10 27.00 55.40 111.00 270.00 550.00 033.00 1112.00 270.00 270.00 270.00 270.00 270.00 270.00 5.50 11.10 27.00 50.40 111.00 271.00 554.00 33.00 1111.00 ta 4.040 4.040 4.045 4.545 4.045 4.045 4.049 4.045 4.040 4.040 4.045 4.045 4.045 4.045 4.040 4.045 4.045 4.045 4.045 4.040 4.045 4.045 4.051 4.0SS 4.445 4.145 4.145 4.04S 4.040 4.045 4.045 4.045 4.045 4.045 4.045 4.045 A r t t 81 ,, C ena, y i t a t MDtnr 10 33 77 133 372 720 1173 1315 1 0 .1 5 MI 1 25 .1 3 MI 1 5 7 .1 4 MM 1 99.00 bb 1 274.74 bb 1 530.90 bb 1 043.01 bb 1 9 4 0 .9 4 bbX -27 -10 4 -11 -1 -4 4 -13 433 1 319.33 bb 15 454 90S 902 775 925 3<1 944 OSO 400 1059 459 379 240 347 324 203 320 151 430 * 1 334.73 bb 1 725.97 bb 1 723.09 bb 1 570.93 bb 1 4 1 1 .7 4 MI 1 244.47 bb 1 497.07 bb 1 420.40 bb 1 442.71 bb 1 740.20 bb 1 330.75 bb 1 279.57 bb 1 192.45 bb 1 270.91 bb 1 341.10 bb 1 150.55 bb 1 140.00 bb 1 111.00 MI 1 323.44 bb 30 -4 32 -13 14 11 41 3 130 391 749 1134 1297 1 1 3 .9 4 MM 1 31.34 m 1 0 1 .9 3 MI 1 1 0 2.30 U 1 200.42 bb 1 552.14 bb 1 035.44 bb 1 955.47 bbX 24 13 11 0 4 -1 0 -14 >i 1 5 -- 0201J* t g u n t l u M b y u l p r i n t d b y k jk U / / l l 000685 Ott 090191t O M B ti U t i kV u p r i n t b y k j k 08/94/91 f W H l i 5r r SS SSKuS g """"" 5SSUU 9 ilglillisf I 3 Iz k & l i i i l s i l i l l ! ................................................................... ? r.*r.rrrrr." ? ? o o uSSSSSSSSSS 3 3 3? . 3 SSS3S Oooo awsawwwwo i O MMV MMM % % V % t f i f S VMM MMV MMM ! o i1 M k S iU tk W U U HUI S.I I f 0 & GO 01 >v- ? Kathod E ilet Last aedU iw lt Compound! P rin ted i Ct \KASSLYNX\PACT*1 .PRO\M ethDR\O2199b.ndb Men Nay 24 0 7 iS 9 s 4 t 11*9 li i m a Man May 24 0 i l4 t2 1 1*9 In carn ai R ef.i Q uantify Traeat Caos, f Standards U s a r MT V a lu si Usar H ak F aeto n I n t e g r a t a Window F a e t o n tMona) 399.00 > 99.00 1.000000, D isaU ad 1.000000 2 .0 0 0 n a ta n tien f in a (mina) R elativ a R etention Tinsi T in e Window (m ina) t Peak S electio n t 4.040, Raablad 0.000, O issblad 0.599 H aarest Raapensa Typst Rospensa B etonai Areas P elyaesdal Typet P o in t e i O rigini P i t Weight i n g i Axis Transform ation L in e ar R x cluda 1/X Mane U nitsi Peak-to-peak aapliC udat -- i n n i i t mi i Window s i s a ( s c e n a ) i JAm b a r o f s n o o th s P ioothing awthedi 114 O issblad 3 2 Jo ln v a lle y threeheld* Reduce peak ta ilin g i R aiaa b aselin a naxiaunt 20.00 100.00 0.00 Draw v e r t i e a l tb ra s b o ld i O aeact sheuldorsi Shoulder threshold 10.00 O issblad 40.00 R elativa h a l i t i A bsoluta h a lg h ti R elativa arasi A bsoluta a ra si 1.50, O issblad 0.00, O issblad 2.00, O issblad 00.00, feab led S p u j} o i o i w ____I C m / ^ y / 9 ? for* 000687 Method R ep art Method f i l e t I n s t m odified P rin te d Ci \KA5SLYMX\FACT-l.PIIO\MechDS\032l9b.i Men May 24 07s994* 1999 2t IS Men May 34 0 0 1 4 t2 1 1999 In te rn a l R ef.s Q uantify Trace Cone, o f Standards U s e r RT V alue V eer Peak Factors I n t e g r a t e Window F a c to r s IS (Rene] TIC F in e d 1.900000, D isabled 1.000000 a.ooo R etention Tine (alas) t R e la tiv e R ten tio n Tinas T in e Window ( n ia e ) s Peak S electleas 9.130. 0.000, D isabled 0.420 Response Types Reopens# t I Polynomial types P o in t e f O rigins F i t W eighting Axle T ransform ations ^ units S xteraal Arena P eak-to-peek am plitudes S m oothing Window s i r e ( s e a a s ) i Hunker e f smooths W snotMng methods D isabled 3 2 J o in v a lle y threshold Reduce peak t a i l in g > R aise b aselin e naxiaust Draw v e r t i c a l th re sh o ld s D etect shoulders Shoulder thresholds 2 0 .0 0 100.00 0.00 ' 10.00 D isabled 40.00 R elativ e heights A bsolute h eights R elative areas A bsolute areas 1.90, D isabled 0.00, D isabled 2.0 0 , D isabled 00.00. feebled J 3 n a o m LAc o s / u f a fiflt 2 000688 Q uatlfy e llM ttiM to pan T0*130-03 d i l a t i ocui crtlteftfelM it ci\M M ttnonncr~ i.9jio\cuxvD a\os3i9k U * t M ditU A t N a a to y M N iN iM U N PrlaC M li Mm t o y 34 M t U i l l I N t ] 1 1 J ] J t i totip 030139t Q a u t l u u by ad pciafcad b y * Jb 09/34/9S 000689 Q uantify C a lib ra tio n lUport 10X120-09 d ilu tio n s C a lib ra tio n s Ci\X XO 0LTXX\W LCT-l.mncurruD\032im Laa t a o d i f l o d i Moa May 34 0 i0 4 t4 9 1991 triatad i Mon May 30 M ilO tSO 1991 a ou 0301991 M a ti ta t o i b y and p r i s t ad b y k jh 05/34/91 000690 AM ELIA062498: FACT E q u ip m en t Log 99016 Q uattro II, #6448E PAGE DATE: 05/25/99 ANALYST: hoi, sah STUDY NUMBER Tox-120. Tox-026 MATRIX: rat liver, monkey sera DESCRIPTION: dils. FACT Method: cts--M -5.0________ Injection volume. 10 uL Cycle time: 9 min. Electrode: Z-Spray_______ M obile Phase: fA12.0m M NH4CH3C02 TN-A- or stndrd number (A ) 99012-10-7 Prepared (date/by): (A) 5/21/99 ias Expires: (A) 11/99______ Store at room temp? [Y] or N Otilen (B )MeOH_______________ . (B) TN-A-2540 (B ) 5/18/99 drb (B ) 11/99 Guard column: None _________ Part number na Lot number na A nalytical column: keystone b c ta sil___________________________________________ Size: 2 x 50m m _________________ Type: c l 8____________ Sphere size: 5 um Part number 055-701-2 Lot number: P7J20 Serial number 038126D A nalytical param eters: Drying gas (L/hrl: 300 ESI nebulizing gas (L/hrl 15 LC Flow rate: 300 uL/min. Back pressure: 70 bar Sheath gas (L/br)J) HPLC solvent gradient: 9min-2 Time (min.) 11 0.00________ 40 2) 1.0_________ 3 4.5 51 6.5 %B 40 95 95 L 1 _______ _________ 71 9 40_ end 000691 Tuning Method Report Method: C :\MASSLYNX\RATS2.PRO\ACQUDB\PFOS Printed: Tue May 25 15:22:53 1999 Page 1 SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. Set Rdbk 3.00 15 5 0.2 150 250 2.98 -15 -5 150 251 Pressures Analyser Vacuum Gas Cell Rdbk 1.6e-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 5 650 7 Set Rdl 15.0 15.0 30 ' 46 2.0 0.0 40 40 0 48 650 000692 tid S _______________________________________________ - M asslynx - Sam ple L ist Sample L is t C:\M ASSLYN X\rats2.PR O \Sam pleD B\052599a.SPL Printed: Tue May 25 15:16:14 1999 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 40 41 42 43 44 45 46 47 48 49 50 ' 51 v 53 54 55 56 57 58 59 60 F ile Nam e 052599001 052599002 052599003 052599004 052599005 052599006 052599007 052599008 052599009 052599010 052599011 052599012 052599013 052599014 052599015 052599016 052599017 052599018 052599019 052599020 052599021 052599022 052599023 052599024 052599025 052599026 052599027 052599028 052599029 052599030 052599031 052599032 052599033 052599034 052599035 052599036 052599037 052599038 052599039 052599040 052599041 052599042 052599043 052599044 052599045 052599046 052599047 052599048 052599049 052599050 052599051 052599052 052599053 052599054 052599055 052599056 052599057 052599058 052599059 052599060 F ile Text methanol blank methanol blank tox120, rbl04199-wblk-1 tox120, rbl04199-lblk-1 tox120, rb!04199-5ppb-1 tox120, rbl04199-10ppb-1 tox120, rbl04199-25ppb-1 tox120, rbi04199-50ppb-1 tox120, fbl04199-100ppb-1 tox120, rbl04199-250ppb-1 tox120, rbl04199-500ppb-1 tox120, rbl04199-750ppb-1 tox120, rbl04199-1000ppb-1 methanol blank tox120, rti, 3M -g1-250 ppb-ms, 4/19/99 tox120, rtl, 3M -g1-250 ppb-msd, 4/19/99 tox120, rtl, 110F-g1-250 ppb-msd, 2/22/99 tox120, rtl, 110F-g1-250 ppb-msd, 2/22/99 tox120, rtl, 106F-g1-250 ppb-ms, 2/22/99 tox120, rtl, 106F-g1-250 ppb-msd, 2/22/99 tox120, rbl04199-250ppb-cc-4 methanol blank tox120, rtl, 81 M -g 6 ,4 /19/99, d1000 tox120, rtl, 8 2 M -g 6 ,4/19/99, d1000 tox120, rtl. 8 3 M -g 6 ,4 /19/99, d1000 tox120, rtl, 8 4 M -g 6 ,4 /19/99, d1000 tox120, rtl. 8 5 M -g 6 ,4 /19/99, d1000 tox120, rbl04199-250ppb-cc-1 methanol blank tox120, rtl, 8 6 M -g 6 ,4 /19/99, d1000 tox120, rtl, 8 7 M -g 6 ,4/19/99, d1000 tox120, rtl, 8 8 M -g 6 ,4/19/99, d1000 tox120, rtl, 8 9 M -g 6 ,4 /19/99, d1000 tox120, rtl, 9 0 M -g 6 ,4 /19/99, d1000 tox120, rbl04199-250ppb-co-6 methanol blank tox120, rtl, 9 1 M -g 6 ,4 /19/99, d1000 . tox120, rtl, 9 3 M -g 6 ,4/19/99, d1000 tox120, rtl, 9 4 M -g 6 ,4/19/99, d1000 tox120, rtl, 9 5 M -g 6 ,4 /19/99, d1000 tox120, rbl04199-250ppb-cc-3 methanol blank tox120, rtl, 1 7 M -g 2 ,4 /19/99, d25 tox120, rtl, 1 8 M -g 2 ,4 /1 9 /9 9 , d25 tox120, rtl, 1 9 M -g 2 ,4 /19/99, d25 tox120, rtl, 2 0 M -fl2 ,4 /1 9 /9 9 , d25 tox120, rtl, 2 1 M -g 2 ,4 /19/99, d25 tox120, rtl, 2 2 M -g 2 ,4 /19/99. d25 tox120, rbl04199-250ppb-cc-11 methanol blank tox120, rtl. 1 7 M -g 2 ,4/19/99 tox120, rtl, 18M -g 2,4/19/99 tox120, rtl, 19M -g 2,4/19/99 tox120, rtl, 2 0 M -g 2 ,4/19/99 tox120, rtl, 2 1 M -g 2 ,4/19/99 tox120, rtl, 2 2 M -g 2 ,4/19/99 tox120, rbl04199-250ppb-cc-2 methanol blank tox120, rtl. 4 1 M -g 3 ,4/19/99 tox120, rbl04199-wblk-1 ________________ ____________________ _ Pagel IMS File In let File 9M IN-PFO S-PO AA -513-613 9M IN -PFO S-PO A A -513-613 9M IN-PFO S-PO AA -513-613 9M IN -PFO S-PO A A -513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA -513-613 9M IN-PFO S-PO AA -513-613 9M IN-PFO S-PO AA -513-613 9M 1N -P F O S -P O A A -513 -6 1 3 9M 1N -P F O S -P O A A -513 -6 1 3 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA -513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA -513-613 9M IN-PFO S-PO AA -513-613 9M IN-PFO S-PO AA -513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA -513-613 9M IN-PFO S-PO AA -513-613 9M IN-PFO S-PO AA -513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA -513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA -513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA -513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA-513-613 v 9M IN-PFO S-PO AA -513-613 9M 1N -P F O S -P O A A -513 -6 1 3 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA -513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA -513-613 9M IN-PFO S-PO AA -513-613 9M IN-PFO S-PO AA -513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA -513-613 9M IN-PFO S-PO AA -513-613 9M IN-PFO S-PO AA-513-613 9M IN-PFO S-PO AA -513-613 9M IN-PFO S-PO AA -513-613 9M IN-PFO S-PO AA -513-613 9M IN-PFO S-PO AA -513-613 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m In-2 9m ln-2 9m ln-2 9m ln-2 9m ln-2 9m in-2 9m ln-2 9m ln-2 9m in-2 9m in-2 9m ln-2 9m in-2 9m in-2 9m in-2 9m ln-2 9m in-2 9m in-2 9m in-2 9m ln-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m ln-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m ln-2 9m in-2 9m in-2 9m ln-2 9m in-2 9m ln-2 9m In-2 9m in-2 9m in-2 9m in-2 9m ln-2 9m in-2 9m ln-2 9m in-2 9m ln-2 9m in-2 9m in-2 000693 \ \ f e s f a _________________________________________________ Masslynx - Sample List Sample List: C:\MASSLYNX\rats2.PRO\SampleDB\052599a.SPL Printed: Tue May25 15:16:141999 File Marne 61 052599061 62 052599062 63 052599063 64 . 052599064 65 052599065 66 052599066 67 052599067 68 052599068 69 052599069 70 052599070 File Text 10x120, rbl04199-lblk-1 tox120, rbl04199-5ppb-1 tox120, rbl04199-10ppb-1 tox120, rbl04199-25ppb-1 tox120, rbl04199-50ppb-1 tox120, rfel04199-100ppb-1 tox120, rb!04199-250ppb-1 tox120, rbl04199-500ppb-1 tox120, rbl04199-750ppb-1 10X120, rbl04199-1000ppb-1 Page 2 MS File 9MIN-PFOS-POAA-513-613 9MIN-PFOS-POAA-513-613 9MIN-PFOS-POAA-513-613 9MIN-PFOS-POAA-513-613 9MIN-PFOS-POAA-513-613 9MIN-PFOS-POAA-513-613 9MIN-PFOS-POAA-513-613 9MIN-PFOS-POAA-513-613 9MIN-PFOS-POAA-513-613 9MIN-PFOS-POAA-513-613 In let File 9mln-2 9mln-2 9min-2 9mln-2 9min-2 9mln-2 9min-2 9min-2 9mln-2 9min-2 000694 S Izs ________________________________ ___ S c a n n in g M athod H a p e rt Method! C:\MMSLYXX\llAT82.Pll0\Acg00B\9MXN-proa-PafcA-513-613 U s t Modified: Tue Kay 23 10:39:4S 1999 Printed: Tu May 25 13:19:29 1999 tolvant Delay ( alna ) : 0.00 Punction : 1 M M of 1 Maaa Pair ( u p - > Inter Channel Delay ( Seca ) : Span- ( Daltona ) : Start Tina ( Mina ) : End Tina I Mina ) Repeats : Channel Parent Daughter 0.03 0.00 0.00 9.00 1 Dwell (Secs) Coll Energy (aV) Cone ( V ) 1' 413.00 169.00 0.30 30 15 Punction : 2 M M of 1 Maaa Pair ( ESP- ) Inter Channel Delay ( Sacs ) i Span ( Daltona ) : Start Tine ( Hina ) : E nd Tina (*Mina I : Rapeata : Channel Parant Daughter 0.03 0.00 0.00 9.00 1 Dwell (Sacs) . Coll Energy (SV) Cone ( V ) 1 313.00 169.00 0.20 30 15 Tuna tion : 3 M M of 1 Maaa Pair ( ISP* ) - Inter Channel Delay ( Seca ) : Span ( Daltons ) t Start Tina ( Mins ) : End Tina ( Mins ) 3 Repeats : Channal Parant Daughter 0.03 0.00 0.00 9.00 1 Dwell (Sacs) Coll Energy (aV) Cone ( V ) 1 613.00 169.00 0.20 30 15 Tunotion : 4 M M o 1 M a a Pair ( ISP- ) Intar Channal Daisy ( Sacs ) s Span ( Daltons ) : Start Tina ( Mins ) t End Tina < Mins ) s Repasts t Channal Parent Daughter 0.03 0.00 0.00 9.00 1 Dwell (Seca) Coll Energy (aV) Cone ( V ) 1 499.00 99.00 0.30 45 60 function > S M M of 1 Maaa Pair ( ESP- ) Intar Channal Delay < Sacs ) : Span ( Daltons ) : Stsrt Tina ( Mins ) t End Tina ( Mina ) i Rapeata t Channel Parent Daughter 0.03 0.00 0.00 9.00 1 Dwell (Saca) Coll Energy (aV) Cone ( V ) 1 427.00 0.00 0.30 40 60 Pag. 1 000695 FACT: DATA REVIEW SUMMARY FORM Date: Analyst FACT Study Number 'y j ' k f T Matrix Time Points Dilutions? ______ 0 Analyte 1: / k & 9' Aecentahfa linear Renee: S T j~g - LOO for ds data se t S ~ lS /y6 Re-evaluated ffardifferent range? Analyte 2: A nSf` 3 Acceotable Linear Range: " 'iS jW J LOO fix'this data set Re-evaluatedfor differentrange? sS _ Analyte 3: /h /7 Acceptable linear Range: vT< -- W /S /h LOO for this data set Re-evaluated for different range? Analyte 4: r*oj Acceptable Linear Range: LOQ for this data set Re-evaluated for different ran^e? j \ J * Analyte 3: Acceptable LinearRange: LOQtr this data set *%0"GVWIURBvIO QZDjCaCQCTmumjmi \ Analyte 6: \ / te i Acceptable Linear Range: ' LOQfor tbis data set \ Re-evaluatedfor differentrWe? ________________________ V - _____________ Analyte 7: \ Acceptable LinearRange: \ LOQ for this data set \ Re-evaluated for different range? \ \ 000636 & oo (? u "I o -SZ. -5 ^ N00Nnt*0 i f I I I H H f l H I C4 I saaaasaaaai sslssss ^3 -"tt rirM OhO A t<-. ?1 2 i IIIn H t H v n aaasas aaaaaaa sSsS 1 H H 1 A No NmO OWWHMAWAfOkW N8 H OH nniHi wA'On V H1H_0f_0#f01s m t4 Wfl*WNh 1H WWW VAAAA nMm4 0kOAW0tA nAO iONoAOo AA rAA*HAo rfAiOrNiOp HiOANONN AA rPOwtA-AOmoOooOoo Oon vA vA A nn OMO ooooooo loeeeoi SWAr*AJoNhoNoo^NoMnf ntfiiAAAAA AMAAAA AA ' AVAAAA IHMOHnAptH r t N A HrtMNOAPAI HH AHMAHttttnH H A A HH Nh AAAAWH HlthMl .fcWMWi ' " 1 t U tj U I |S ..&..............!.................................. _..... ................*....... S *ii3 3 3 31U33_^_ - 3 3 8 ii!l 5 3 !ii3 8 s3 ls8 ls2 Iil8 3 l3 lilsl3 3 l;M IIl!f j) OooOooOooOooOoo OooooOooOooOOoo oooo oo oo oo oo AAAAAA 33335 333333 vrvjU i i i i StStSB kiiIAAAAA Ao mo ni nimi ni aS SAAHASAAHASAAAH.AAAHSAASAHUHIUI NHAotiA0AHNiAmHNiAOmHNkAmar^tIIPu0i A010A1001t0011NI k k * _>rt o m m m m m - 01 01 01 01 01 01 f SSSN SN U HHrt4 I NSSSSN*VWsWNWS ffit 01 0k 0k 0 01 01 U H 4 H H H H I 01 0k 01 0 0k 0k N ssssssU0 0) 0k 01 01 0 I 0 1 0 0k 0k 0k 0k U 0k Sr-tHHrtjw^* Ht ftftftft 2g2aSn.&saLsAi 1".t.".t.7.t..M.. S 35+S& S A m * * &S^HMomJ'IdJ11I4oAAMHf1f*fAAoHMi4TAMoAiAoHAiAHo?iAAHo;AiO#Ah0m4A0AhNm3mQH04hAM)r4A0HAhM3O04A4h-M)tH4MRHNxOII*HzNoOt.IhtHIHOwhOHHbJ**oWbMHnJoHWHh|*OmHa>AmNIo. WWWA BIAAAAN . - . *o A*A*A*A*AJ.AAI * AAAAAN NNNNN eiene^ AAAAH4h s h g h g n g n * 4HHHH.OH. UMMMMJ**J*44343 ` b h MMh h 3si r..i.H..H...W...H...HNHoNHo.NHoNHo*NHo*acooNNo No No NO NO ONj o N o N o N o N oo NN eo o oo oo jN N N N N M ! * O O O O OO B HH H 4hN N N N N S N O NNNNNNA *O A O j0N A A A A A A N A ) H A H N A H 01 P - H n h soHi 4MBmHhiHshHhNguNgkNnHnsJkhs*OI0..W03.HHjS*HH0aoH1oHJoaHotHHAaooHraOoH4t aAOoHH aJOorik-4o**Ot Ho00oIk1Hrooo0rIH4koo>00rIkkHoo40<0IkHk 43 43 434) " Mh H H Qk k k k k k k k goooooooo` S o o o o o o o J N N N N N N N N N N N N N N N fS fl SI _.x m x x v x x x x x k x I j x x x x m m S x x x x x x S xK xX xX xX x 4s ? a s 4Q>O 4Ol0t i480 IOJO4 UO1Q0 QO >0O4 UO<O OM <OUO4 49P4 OMOW 0O4Ol 0O0U OlOk )O4Q} kQi0| g g gSg S 41 AJ AJ U U *4 f8888S88 fgggggggg |0 4 l0 0 4 l 4 4 tf iSSS 41 AJ 4J 41 3O0001kO0OOkkOOOOkkOO0OkkmooOOkkoo00wk1f0oO0-kkOOo0OkkOoOOOkkkHoo0OkkHvo0O-kitNO0Okk-O0OAkk-<Ii4MkkA0AoiH0AkoHOrAokH0AAokMOAoOkN0AoHiN0AokNNOAoknN0Ao<kN0oArkANo0AkNOWOOkkOONOMkkfcc< IINA NA NmNa 0>m iAA OO A A I I a a a a a a a a a a a AA* >OoII>Nm Nm ' iII N A N A N A N A N A N A N A N A N A N A N A NNf AAH o o o o o o o o o o o o O< HNnoAWhwAOHNnAWham( No0kmo0kfio0kj-ipo0N1)noOnkno0okAcOojkpo0koor0k B--A->kOOokHoO-kNoO-kAoOkOO--AO-W-O--PoO-kO-0o-kA-<t-O-o-r-o-I Mkfo0<kmAOok oOmkoOmmkoOtAtkrAoO-kcAoOoAkooOWkkoOOWkorOAWkoONWkoOrtkcU^fl Om10Om10o Ok Ok Ok o Ok O Ok o Ok OkCk O 0k o 0k 0k mm >mmknm mmmminmmmmmmmum m AA A A A NN NNN N N N N mm *mm mm mmm m m m m m m Oo ooooo<oooo<oo ooooooooooooooo o o o o i 0k 01 Ok Ok Ok Ok Ok 0k 0k t !0k OkOk Ok OkOk O k O k O k O l O l O k O k O k C m m m A A A AU I N N N N N N N N N f N N AN N N N AAA mOk mOk mOkmOk Nm mN OO Nmo moN iwr-oAOHNAvAWACtComv-ii NOC 7%. <D C> O O o a * 1 e L 3 XXf Anali 062499: quantlatad and printad b y boj 5/28/99 J a u i* u m h ( *uiui m uiV uu><(Mu 9 10 40 40 40 40 40 40 40 40 40 910O 4O0 4O0 4O0 4O0 4O0 O40 O40 O40O10 O IA tt j0 b lA W M H O (0 :HO(oa>Joiv*WNMOttBg ilU U U M M > itMHOWM^nUtBWMHOWO^aWAi m tuut> 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 M H M JtO l lU K jU JlU tU tU l i iU lM n U ltM M ll )N > M M M M N M M N N N M N N M M M N M M M M JIU U IU IU IU IU IU I t IU I tU I Ib lU llN IU llll tMuMMuKu) w u <0 m OOOOO OOO OOOO M M mM MuiMm M(p Mw Mc p Mw Mw M0MmMu UMUMIMMMl 4P u* ui ui m 10 10 4M U U U t U t U t U t t u u t m ut Ow Ow O10O40O(0O(0Oin M NNM M M M U t Ut ( 0 040 t u u > 4 0 40 40 40 40 40 40 40 40 40 40 40 40 40 1 0 0 4 0 4 0 4 0 4 0 4 0 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 ( A 40 40 ( 0 ( 0 10 40 40 40 40 O O O O O O O O O O O 0-0 O O O O O O O O }l0l^UMHO(Da'JAU*UNHOVO>J uO wO Ou Ou Am *u O u O u UO MO KO) OK IOMOMOMOM O O O OOOO OOOO O 40 O 4 n u 0 U K t H 0 4 0 W A U * U U O O O O O O O OOOO MMO O OO O M O 40 CB J 04 40 rt rt rt rt r SSS85 ft ft ft ft ft ft ft X ft rt rt rt rt rt rt o p o p o p o aopooooo_ gs ft ft ft ft ft OOOOO ftrrrtftftftH rtftftftrrft O O O O O O O O O O 0.0 O X X X X X X K Q X X K X XX - X g t Si r .X....X....X....X...X XH MX HX HX HX HX tf trXHXH XH XM XH XM N 0 U 0 N 0 N 0 M 0 0 N0 N9s0 M 0 M M N N N M IM N M M 0 0 0 0 0 0 9 OOOO M O 0 MNNMMN g OOO OO O - - * * * % * * * % .......................... o H H 1 M! HS' H0*0H* tHr<4 H H H H K H t| tr tr tr tr tr tr rt t 00004o o o o o o*> I 6 Xa a a M M M M M M M t Htr Hft Hrt Hrt f* ti rt rt H er tr rt H rt H rt * rt h ft H rt t O t t t t t p h0o *h h% h* h^ h m ia o * % * * a- 9 * H N N N 4 J H H }fH N N M H H H K 'H V t0 l0 l0 t%r tr r1t fHt rXt Xrt Xft tr Htr Krt HrtNftHrtHrt HHHPHHH g o .**** h0 0 5 2 ........ X h a a a 0a SSSSS! SKSSSS g g SI 4 0 40 40 40 40 40 4 0 M - > i p | p 40 40 40 40 j 4 I0 N M U 4 H 40 ? w p t r o ' u S S a.H I i I I iT i MlO 0 0 1 0 0 0 IP M N M N m m lilil I I I IT WUol004001004O04 mm g 04 04 04 04 04 0t SHSHSHS HNH. HS n 40 40 40 40 40 40 fIf HWH Ms SH O 40 40 40 40 i a a 4040 a I 40 40 40 40 40 ftft U4 U 414 U U4 U4 OOOO OOOO 0000 AM nMaHoH. Ha OOOOO OOOOO OOOOO aH Ha Ma Ha Ha OOOOO OOOOO OOOOO Ht r cHr Xc rHt rXc rHc rHt r t r t r fat H H PH H H H H H o o o o o o o g g I 40 40 40 40 40 40 40 40 40 40 40 40 40 40 I I I I IT I M UNM UHI 0 0 0 0 9 70' ilf? ft | Ck in r s - f ih i iy tit2 s ? " I K. B * B -3 ~ 3 3 H M> 40 X 40 Ti 56 pm euN M U M o JH M H H U a b h o w h ip 0 taU>UMPUM0 (0 auuuuaui UCt A H O H N u t w o u u* m u t H IO H B M O U A U I0 U M O <J Ol J*I0 U N H hm m m hh WOAUUMU U A H ^ B 0(1 UHMHH MAH0UA40 HH H N *JH H I0 C H NH H 00U 0A H O0M 0AH0 A H H H *JH U O in *J O O % gSS&gSg gg&5?gS 5 till M UUOA MUON NOAI AW OO BC. . . . 1 g^a a a H B 4 IM H H U U l-jM U lM I' M u a a P i- 4 1 as. t*U lU lU IU IU IU M JJIO lU IU M 0U IU *00 U00 000v00)040f0*U*rM<Ao4Uua0wa*uw*ia0aA00a*a* 0HJ M ilk W 4P H WM 0 gg 1 H *m m m h h M m 9 40 <D 04 HI 40 ! W W M N 0 0 H U > IH 0 U * iM 0 N 0 U a O A O N N 4 0 O W V iU 0 U l4 0 U iH a A A * l0 1g&ggffggg g g g g g g g irv < ? 11 i r UT M l 1H H U U " St v/ 0 8. 3 m IQ ?2 3 ? Quantify Ccaound Summary Raport TOX-120 Xat Livar Dilution 8ampia U a t : S:\PACT-1.PRO\SamplaOB\051499a Last aodifiod: Mon Hy 17 14:14:20 1999 Mathod: S : \ P A C T - 1 .PftO\>totb&B\051499a Last aodifiod: Mon May 17 14:23:30 1999 Job Coda: Printed: Tu M ay 1 08:22:40 1999 Compound 2: M463 4 Mua 1 051499041 2 051499062 3 051499063 4 051499064 5 051499065 6 051499066 7 051499067 9 051499068 9 051499069 10 051499070 11 051499071 12 051499072 13 051499073 14 051499074 IS 051499075 16 051499076 17 051499077 18 051499078 19 051499079 20 051499080 21 051499081 22 051499082 23 051499083 24 051499084 25 051499085 26 0S1499086 27 051499087 28 051499088 29 051499089 30 051499090 31 051499091 32 051499092 33 051499093 34 051499094 35 051499095 36 051499096 37 051499097 38 051499098 39 051499099 40 051499100 41 051499101 42 051499102 43 051499103 44 051499104 45 051499105 46 051499106 47 051499107 48 051499108 49 051499109 50 051499110 51 051499111 52 051499112 53 051499113 54 051499114 Saaplallst Taxt MsOH Blank MoOH Blank . Tox-120, RBL04199-H20Blk-2 4/19/99 Tox-120, RBL04199-LBlk-2, 4/19/99 Tox-120, RBL04199-10ppb-2, 4/19/99 Tox-120, HBL04199-2Sppb-2, 4/19/99 Tox-120, *BL04199-S0ppb-2, 4/19/99 Tox-120, RBL04199-100ppb-2, 4/19/99 Tox-120, RBL04199-250ppb-2, 4/19/99 Tox-120, RBL04199-S00ppb-2, 4/19/99 Tox-120, RBL04199-750ppb-2, 4/19/99 Tox-120, RBL04199-1000ppb-2, 4/19/99 I M S Blank Tox-120 23M G2 / Dl:23 Tox-120 24 62 / Dl:25 ' Tox-120 2SK 62 / Dl:25 Tox-120 26M 62 / D1:2S Tox-120, RBt04199-2S0ppb-CCl, 4/19/99 M.OH Blank Tox-120 33K 63 / Dl:23 Tox-120 34M 63 / Dl:25 Tox-120 35N 63 / 1)1:25 Tox-120 34M 63 / Dl:25 Tox-120 37M 63 / 01:25 Tox-120 38K 63 / D1:2S Tox-120 39M 63 / 01:25 Tox-120 40M 63 / D1:2S Tox-120, BBL04199-250ppb-CC3, 4/19/99 MeOH Blank Tox-120 27H G2 / 01:10 Tox-120 29H 62 / 01:10 Tox-120 30M 62 / 01:10 Tox-120 31M 62 / 01:10 Tox-120, BBL04199-250ppb-CC4, 4/19/99 HaOB Blank Tox-120 4211 63 / 01:10 Tox-120 43K 63 / 01:10 Tox-120 4SM 63 / 01:10 Tox-120 46K 63 / 01:10 Tox-120 47K 63 / 01:10 Tox-120, RBL04199-250ppb-CC3, 4/19/99 MeOH Blank Tox-120, HBU)4199-H20Blk-2, 4/19/99 Tox-120, RBL04199-LBlk-2, 4/19/99 Tox-120, RBI,04199-- 5ppb-2, 4/19/99 Tox-120, RBL04199--10ppb-2, 4/19/99 Tox-120, BBL04199-25ppb-2, 4/19/99 Tox-120, BBL04199-50ppb-2, 4/19/99 Tox-120, BBL04199-100ppb-2, 4/19/99 Tox-120, RBl,04199-250ppb-2, 4/19/99 Tox-120, RBL04199--500ppb-2, 4/19/99 Tox-120, BBIt04199-750ppb-2, 4/19/99 Tox-120, RBL04199-1000ppb-2, 4/19/99 Typ* Analyta Analyta Analyta Analyta Standard Standard Standard Standard Standard Standard Standard Standard Standard Analyta Analyta Analyta Analyta Analyta OC Analyta Analyta Analyta Analyta Analyta Analyta Analyta Analyta Analyta QC Analyta Analyta Analyta Analyta Analyta QC Analyta Analyta Analyta Analyta Analyta Analyta QC Analyta Analyta Analyta Standard Standard Standard Standard Standard Standard Standard Standard Standard Std Cono XT 5.56 11.10 27.80 55.60 111.00 278.00 * 556.00 833.00 1111.00 278.00 .5.307 5.306 ` 5.307 5.307 5.306 5.308 5.308 5.308 5.31S . 5.307 5.306 5.307 278.00. 278.00 5.308 5.306 5.307 5.307 278.00 5.306 5.307 5.306 5.307 5.306 5.56 11.10 27.80 55.60 111.00 278.00 556.00 833.00 1111.00 Aras Kaoponaa Cone, rings %Dav 613 637 509 ' 473 612.731 636.927 509.037 472.806 48 49 47 44 44 35 64 43 48.048s 48.381 46.922 43.598 43.676 34.651 44.313 42.794 1080 1367 1207 1023 1079.684 1367.145 1206.705 1022.573 66 66.125 83 83.086 50 50.209 63 63.197 55 55.155 bbx bbl bbX bbl MMX MMX MMX MMX lfifX MMX MMX MMX bbl bbl bbl bbX MMX bbX MMX MMX MMX Pag 2 Soup 020199, Xaviaaad and quantitated by drb 8/17/99 000699 Q u an tify Compound Sunaary la p o r t toxl20, r t l ampi. Lit: C :\ M M L Y N X \ r t 2 .PKO\bnplaDB\OSZS99a Laat modlflad: Wd May 2 07:17:2V 1*0* Mathod: C:\MMaLytOC\rata2.VlW\MathOB\OS2S9Sa Laat ediflad: ad Ma y 2 07:10:17 1900 Job Coda: Printad: ad May 2 00:20:32 1000 Caopound 3: M613 1 HtM 1 052599001 2 052599002 3 052599003 4 052599004 5 052599005 6 052599006 7 052599007 9 052599008 9 052599009 10 052599010 11 052599011 12 052599012 13 052599013 14 052599014 15 052599015. 16 052599016 17 052599017 18 052599018 19 052599019 20 052599020 21 052599021 22 052599022 23 052599023 24 052599024 25 052599025 26 052599026 27 052599027 28 052599028 29 052599029 30 052599030 31 052599031 32 052S99032 33 052599033 34 052599034 35 05259903S 36 052599036 37 052599037 36 052599038 39 052599039 40 052599040 41 052599041 42 052599042 43 052599043 44 052599044 45 052599045 46 052599046 47 052599047 48 052599048 49 052599049 50 052599050 51 052599051 52 052599052 53 052599053 54 052599054 55 052599055 56 052599056 57 052599057 58 052599056 59 052599059 60 052599060 61 052599061 62 052599062 63 052599063 64 052599064 65 052599065 66 052599066 67 052599067 68 052599068 69 052599069 70 052599070 Saaplalist Tant nathanol blank Mathanoi blank toxl20, rbl04199-wblk-l toxl20, rbl04199-lblk-l toxl20, rbl04199-5ppb-1 toxl2Q, rbl04199-10ppb-l toxl20, rbl04199-25ppb-l toxl20, rbl04199-50ppb-l toxl20, rb!04199-100ppb-l toxl20, rbl04199-250ppb-l tox!20, rbl04199-500ppb-l toxl20, rbl04199-750ppb-l toxl20, rb!04199-1000ppb-l aathanol blank i\fc? tox!20, rtl, 3H-gl-250 ppb-as 4 / 1 9 / 9 9 | | eC toxl20, rtl, 3K-gl-2S0 p p b - u d , 4/19/90 toxl20, rtl, 110r-gl-25O ppb-ma/, 2/22/99 toxl20, rtl, 110r-gl-250 ppb-aad, 2/22/09 toxl20, rtl, 107-gl-250 ppb-ma, 2/22/99 toxl20, rtl, 10F-gl-2S0 ppb-aad, 2/22/00 toxl20, rbl04199-2S0ppb-cc-4 nathanol blank toxl20, rtl, 01M-g(, 4/19/99, dlOOO toxl20, rtl, 02H-g, 4/19/99, dlOOO toxl20, rtl, 03M-g, 4/19/99, dlOOO toxl20, rtl, 04M-g, 4/19/99, dlOOO toxl20, rtl, SH-g, 4/19/99, dlOOO toxl20, rb!04199-2S0ppb-ce-l nathanol blank toxl20, rtl, 0K-g, 4/19/99, dlOO toxl20, rtl, 7M-g, 4/10/09, dlOOO * toxl20, rtl, (8K-g6, 4/19/99, dlOOO toxl20, rtl, 9K-g, 4/19/99, dlOOO toxl20, rtl, 90M-g(, 4/19/99, dlOOO tox!20, rbl04199-2S0ppb-ee-S nathanol blank * toxl20, rtl, 91M-g(, 4/19/99, dlOOO toxl20, rtl, 93M-g, 4/19/99, dlOOO toxl20, rtl, 94M-gS, 4/19/99, dlOOO toxl20, rtl, 95M-gi, 4/19/99, dlOOO toxl20, rbl04199-250ppb-cc-3 nathanol blank toxl20, rtl, 17M-g2. 4/19/99, d2S toxl20, rtl, 18M-g2, 4/19/99, d25 toxl20, rtl, 19M-g2, 4/19/99, d25 toxl20, rtl, 20H-g2, 4/19/99, d25 toxl20, rtl, 21M-g2, 4/19/99, d2S toxl20, rtl, 22K-g2, 4/19/99, d25 toxl20, rbl04199-2S0ppb-cc-ll nathanol blank toxl20, rtl, 17M-g2, 4/19/99 toxl20, rtl, 18M-g2, 4/19/99 tox!20, rtl, 19M-g2, 4/19/99 toxl20, rtl, 2QM-g2, 4/19/99 toxl20, rtl, 21M-g2, 4/19/99 tOX120, rtl, 22M-g2, 4/19/99 toxl20, rbl04199-250ppb-cc-2 nathanol blank toxl20, rtl, 41M-g3, 4/19/99 toxi20, rbl04199-wblk-l toxl20, rbl04199-lblk-l toxl20, rbl04199-Sppb-l toxl20, rbl04199-10ppb-l toxl20, rbl04199-2Sppb-l toxl20, rbl04199-50ppb-l toxl20, rbl04199-100ppb-l toxl20, rbl04199-2S0ppb-l toxl20, rbl04199-S00ppb-l toxl20, rbl04199-7SOppb-l toxl20, rbl04199-1000ppb-l Typ Analyta Analyta Analyta Analyta Standard Standard Standard Standard Standard Standard Standard Standard Standard Analyta Analyta Analyta Analyta Analyta Analyta Analyta QC Analyta Analyta Analyta Analyta Analyta Analyta QC Analyta Analyta Analyta Analyta Analyta Analyta QC Analyta Analyta Analyta Analyta Analyta QC Analyta Analyta Analyta Analyta Analyta Analyta Analyta QC Analyta Analyta Analyta Analyta Analyta Analyta Analyta QC Analyta Analyta Analyta Analyta Standard Standard Standard Standard Standard Standard Standard Standard Standard Std Cono 5.56 11.10 27.80 55.60 111.00 278.00 556.00 833.00 1111.00 278.00 - 278.00 278.00 278.00 27B.00 278.00 5.56 11.10 27.80 55.60 111.00 278.00 556.00 833.00 1111.00 Kt 5.795 5.797 5.765 5.808 5.784 5.782 5.776 5.767 5.788 5.782 5.778 5.784 5.772 5.765 5.767 5.767 5.792 5.782 5.795 5.781 5.813 5.812 5.791 5.788 5.815 5.783 5.785 5.782 5.789 5.741 5.807 5.806 5,775 5.786 5.790 5.765 5.787 5.786 Aran Cone. Flags %Osv 3 1.54 KM 5 8.66 MK 14 32.23 bb 33 82.54 bb 53 137.72 bb 116 304.34 bb 221 587.57 bb 318 848.84 bb 369 985.61 bb -72 -22 16 48 24 9 6 2 -11 105 274.93 bb 118 310.32 MM 104 273.67 M M \ 92 241.88 M M 2 102 268.45 bb < w e r e c l 120 315.53 MM J 101 266.49 HM -4 112 295.72 M M 6 112 295.27 M M 6 100 262.77 M M 5 8.69 bb -5 76 199.37 MH -28 . 36 89.73 M M > 28 69.25 b b :/ i 1 33 84.01 bb *) E i i fcru 30 73.71 b b < 39 96.92 bb ) 29 72.66 bb > 81 210.54 M M " 24 27 66.29 bb 9 17.56 bbX 216 x 7 11.87 bbX` 7 13 29.34 bbX 6 11 23.51 bbX -58 41 103.06 bbX -7 87 227.94 bbX -16 150 398.05 bbX -28 204 542.63 bbX -35 252 669.29 bbX -40 Vag 3 Uc. oil Anali. 0(2490: quanti atad and printad by ho] 3/2/90 000700 sP Ift i I 9 t S 0 0 0 0LA MKAAA A( lA A U M H f It ffllAV Ui gMiHeitt tDMAf^lAA AMAAAUANA AH AOAlAll IAU M H O VA>JA AU M H * > 0000 lu m u ib i (M M M M i m m m ui > U M O U > tO ) 10 40 0 IA > 0000 IAAA A M P lA e o o O O O O O O O OOO OOO O O O < O O O O UO(A AAN M U----U--MU AAAAAAAAAAUJ IA Al AIA AAK) IA IA 4AIA IA AAAAAl AIA IA l AIA t n (a I A I A _ _ _ _ _ _ AIM M M M M M M A IM M UUiA IA IA U UH* CAIA IA IA IA 04 IA Ui Ui IA C IA IA IA IA4I'A IA *04' IA" I"A *I" 40 IOIO40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 If 40 40 40 40I 40 40 40 40 40 4 40 IO40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 If OOO O O 0 0 0 0 0 OOO OOO O O O C 40 40 40 40>40 40 40 40 40 4 O O O o> 0 0 O O O I A A A 04 04 01 AAU O IO A IAIAIAIAC(AACUA>01 (A *A A M H O I0 O < J A IA *U M M O WWW! 40 00 J < IA M (A 40 40 O u IA M (A 40 40 O u OOO IA IA (A MMM (A IA IA 40 40 40 40 40 40 OOO uuu U K1K OOOO IA IA IA IA MMMM |n <A<AtA 40 40 40 40 40 40 40 40 OOOO MM MM O 40 CDI OOO O O O O O O O CA4AIA IA IA (A 4AIA IA 4A M Al N M M M M M M M IA IA (A IA CACAIA AIA IA 0* IA IH IA 10 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 0 0 0 O O O O O O O OO O O K) A) Al N N N N H H H 01 IAUAAl> H O IO B J O O i A U OOO IA (A (A M Al Al IA IA IA 40 40 40 40 40 40 OOO MHO IA 40 40 O O 10 IA 40 40 O O 00 O IA IA MM IA AIA 40 10 4 0 40 40 4 0 OOO Oo o *4 04 O IA 40 40 O o O IA 40 40 O o O t 41 < < O *" rt rt rt rt rt 00000 M X X M I HHHM Isssssssir rt f t f t f t f t ft X r t r t f t f t f t f T f T l OOOOOOO XXXXXXX Bm m m m m m m S oooooooa 5 ilil _*I s s s s s s s shi r t f t r t f t f t ft X f t f t f t f t f t f t X 1f1t f t f1t f t f t f t f t g f t f T f t f t r r r r r t f t O O O la m a s x S k S S S x `T H H H H H P H M H M M M VM M AB M M M M M M >5 O O O O O O f t MMMMMM 9 OOOOOO B9 M o M o M o M o M o M o M o ft a o M0 M0 M0 0M 0M 0M 0M 0M 0M 0M 9fOt Of?t f0ftt* **H H U H N H H 8O' f t f t rr f t rt f t W f t r t r t r t r t r t l l^^***ftft*ft*ft-*ft*ft g o -------------------------------g o ---------------B2 .............B s s s p p s s r TIf H f -- .*1 H N H H t O' IT f t f t f t f t f t -ip H H H H H KHIBOOOAlr f f f f . T I I 7 I I I IIM M M M M 8 e a 9 i0*i0oi rOr'_O 40 10 40 40 40 40 ssssn W S S S S I 10 40 40 40 40 40 N I) l iQ IA M Al Al M M M $ .................................. V A *A A A * ffS S S N S S IH H H H H H O 40 40 40 40 40 40 ft S S S S S S i 40 IO 40 40 40 40 S AAAA I H ftftft 40 40 40 40 I 40 40 40 40 IA * 01 04 04 04 40 40 40 40 40 MO O O O O |A 04 04 04 04 04 1 ft*ft*ft*ft*ft* fftt S40 S40 S4 0 S40 S40 I 40 40 40 40 40 tr *ertr o* tr tro' tr XtrXcrXo'erer fftt ^ p H f t f t f t f t f t f t ***** ` OOOOOOOO XaJ Mafo| o44T 1T0 n r 7 7 r ft* ft* u o a fttO I I O ft* ft* ft* ft* M M " I I I I In IA MMMMOO 4 0 4 0 40 40 40 40 40 40 40 40 40 40 40 40 40 ft*-J(AA>ft*tAAft* O' O ' O ' I I I I l I H H ft* M 10 40 40 40 40 40 4 0 40 40 40 40 40 M 40 40 40 40 ft* 10 40 40 40 40 fcfcft&fcfc IA CAIA 4A4AlA aM aH dH uH OOOO OOOO 0000 aftnHaMa ffttft OOOOO OOOOO OOOOO aft*aft*aft*aP aft* O0 0O O0 O0 O0 OOOOO M SM M HV SM SS40S MMNMNU M V. Al M 40 40 W V S ID 10 40 40 40 40 40 40 4? I > i|U im i III? ft* ft* CD CA M f t * ftU (R < JM lA N H ft*U 049ft*CA 4ft*CA OOOOOAAM U OOOOOOOOO M vl CD O O M 4 O O ( A ( A CA I A I A t A I A I A CA (A IA CA CA CA CA CA CA CA IA m m m m m m m n w * 1 0 IO 0 A i* J O O JO V M A M * I0 U N M W UW MMMM M O O 0000 * UUOW HAM M CD M MM M M <J J 1 A CD CD od m OO OO 00 00 ft* ft* m CA M f t * ft*M CAJft*CAM ft* t*M 0lCBft*CA'4ft*CA O O O O O 0 4 C ft* CA 0000000004 CA t A CA M M OI CD 40 O 0*0 CA ( A CA (A CACA CACA CA IN | A (A M M M M Al Al Al Al Al Ai M M CD 40 J Oft D U < l < i 40 J 0k CD CD * 40 W A M U 0 CA * O CA CA CA (A CA CA CA I A CA CACA CACA CACA `M M M M M M M M M M M M M M 0 0 0 0 0 * 0 0 4 CA 0 4 * J 04 1 * C A M M O O D C A M ft* CA 04 O 0 4 CA CACACACACACACACACACACA MMMMMMMMMMM <4CD0ICA<4<4CAO404CDM C B *4O tA -4O D 4O *M 40 i o m ca m m O 4O M 04O CA A M M U O O U C A *J < I O V f t O 01 1 * l A I A CA 01 01 O ft* 40 M 4 0 * Oft Ak * JU A M A l CD M ft* 4 0 U f t * H M H * 4 * jA ft* 0 0 { A M O 4 (A 0|40I0M O O A A O 0< J< 0M < JO O M ft* Al ft* ft ft M M M 40 ft* 04 M M O M * 40 O 0 k CA M 04 * 0ft 01 CA 00 J CD M O * * w CA m m m * * * . 2 I I I I I I t Ift* U U X N ftW *A O VOAHXW AAO 311 370 367 279 ft* 0k A Oft sm t*l * * * (A Ol 01 CD O <J 04 01 U - J 40 40 * 0 01 04 * IO * 0k 0k * 0k U 9 CA CA 0 4 0 4 04 * O 04 O 40 40 04 * O ft* 04 M O 40 U 4 4 0 O * M f t * C A O 04 04 Ot M * 04 ft* ft* M ft* 9 * ft* ft* M ft* 0 4 * 40 M 4 0 * * l 0 f t * JV 0ft*IA 4A 40M M M *M OOO . 00 OOO 88% M MMMM MU M* * * CA (A O ft* CA O * 40 0k a 0 A 40 0M M 01 O 4A CD M C A 40 ft* * O ft* U O * A * 40 M J A CD M CD ft* Al O A 04 A CA 04 M 88888888888 M * * M (A M M U M * * 4*1 Iti CD CD M * O * O CA 0 4 CD CA CA (A O M 4 0 O O 0 4 O 4 4 CA O O 0 4 O O f t * O M 4 0 0 A Ok M O ft* O M 40 0 4 f l D C A J O O * U 4 | A CB O 4 88888888888888 4 0 CD 0 t M ft* CD M M ft* M 0 4 * *IA C D O O 40 4 -* * M O O IA **C D O A 4O 0k*O O * M 4 0 IA 0 4 W ft* 0 4 O O O S8888888S88 t- 1 0 0 - . I ?r 0 "C5" r* I tI ft* I ft* ft* M in IA M ft*ft*MMflU'ft*CD40 3 I n< Vnn0 nnh H <H 9 Hi V 0iOr t f f t H wi H 00 00 Na H0 N f ii i iiii o* s sssssssss s s s OHHHHHOHOOO MOOOOH m r* n N n n n N W N H 0 O h O A O 0 2 NP><monH0Nt' OoVAOrintf ft A 0 * n n f 4 o e H-1N H N N N K 1 AH NV NN AA AO NN mA nA nA H0 AAnA OOAOOAAAAAA 1A 1A 0 1 A 1A 0 0 0 0 0 0 HA HO NA AA OH AA 0A AOAAOAA 0M00M00 n a a r- on AAAA0AN IIIIIII nIAIn AAI AAI AAIAAIHAI. DIPwlIlnH nH HIAIN NI ArINtI*HI4N!mH 2 2222222 2222222 222222222222 o o o o o o o 0 0 0 0 0 0 000HOOHOOOOO f00Nm in n noa a>A 0 O A N r* OlAHA A N A M A A HOAnPIOAHAAAA PA0A0AO H 0 O 0 N N N N O O A O OAH0AWO HNtHHTN OOOOOOO IO A A A A A A O000A0N NNHAHAH OOOAOAO MHhNAAONrHNH AOHNH0OAAAAA AOOOOAOAAAAA IAAA0A00000 ss.... h h h h .........._ _ J 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 SSSSSS SSSSSS SSSSS OT*0TJflTJtTJ*0 h U titih titi H n h h U U H H h U U U h ^ & h iU ih i <r* "3 2* AHNNS <0 VT9 T) 3332 OOOOO OOOOO OrjO O O O OOOOO OOOOO OOOOO OOOO OOOO OOOO AAAAAA AAAAAH AAAAA I AA AA AA AA AA AA nI A A A A A H AAAAA0 SSSSN.S 0 AAAAAA P HHH I HHHHHT HHHI HHHHHH1 O O Nn Nn nN AN Aa S.-s*S.N.'*s< s s s A n n s s s n J SSSSS.S 000ft 0 0 0 0 0 0 1 JAiA'l nnnnnnftOA O O n s n a 0 a i i i iS N1 NI HA HAH0H*0OA O <0O O A A A :i y AAAAAC4 AAAAAn A AnA H N A H N A h H H H I IJJ N A Mh1 1 * 1 1 1 1 1 1 AAAAAAAAA A Am kwh I IX O O A A A ........ A AAAAAAAAA ZZHHOOA. RRh h h h h J 90000HM 0 0 0 0 " O O O O O O O O O .. 0 3 a0 5 a0 A .y.1 SA A SA SH X H sH HSn iN Sn.n. x .ss HaHaHNaaNnan^0nAIH,AA9fIlHAAAHIAASIHAAoINAAAI AA0HI0AANI(AA0I)AA0IPAA0*IAA0HI t . . OS OOOO O O O O O O O O O H.p H H-OHA H k H A H A HH J A H A h h h h h h h h h h h h h h h h h h h h h h h h h h h h h h h h h h h h h h h h MHHUUUU * sssssssssfssgssgsissssssssssssi ggggg^ggggggglO O O O O O CitiCiCitiCi c2 OnOnOnOnOn OnOntOntOnkOntOnOnkQ<L0nk-n0knOknOknOknOknOk Oc0 k S XX*MMMAJ. . H H H H H H H H H H H H H H H h HHHHHHHHHHHH,S h h H h h x h h h h h h h j HHHHHHHJS IAsJs3 i*J J *J *J*J +J J 4J44I4J40 4141y 4JilililJy y0 y0 0y 0y 0y 0y 01 AxoJaoxJaoxJAoxJAoxJJoxJAoxJoAxJoAxJSAxJSAxJSAxJ 1 nnonnhnnnh H>> N00 00n 000 mO Ow Oh ooO0 ooO0 oOH 1A 0101 AAA A A A A vt00A A A anAO nOaA nOaA nOAa nOaA OnAa OnAa AA nn AO OA M H o A A N n0O O o oo A A AA AAAA AA nA An 0 O A A An 0A i* O A A nA 0A A O< A< A( An * 0At 0 A A A A 00 AA AA AA AA nnn AAA0 0AAA 0AAA nA nA An OOO 9 n b iIiiii>Ii1i)>illnAAAnA00 A00nAAnA AnoAAA A A An oA H N PIT A o r*O A AAAA AA OOOO 000 O O AAAA AA AAAA AA An An AnAnAnnAnA inn C4C AAAAAAAA A OOO OO O^ n^ n9 A0 V0 A0 O0 n0 A9 A0OArA AAAA0A>AAAOrA *A9AA ------o--o----I--o--o------>--o--o--<--O O O O O O O O A A tA A A A C A A A A A A A A A A AA A A A A A A A A A A m tnA A iCif4fiCi AAAA OOOO >i}>OAAnnOAA o___o)1iAAonnAoAMc AAAAAAAA nnnnnnnn AO AO AO AO AO AO AO AO ihn A A r- m A O I w w 0A A A A A A n >00 AA O A O A OA OA O A O A 0A 0A AA A A A A A A A A )A in A n An An An nA A A AA AAAA OOOOOOOOOOO 33 Hnn000p HO dH HN Hn H0 H0 HW Hh H# H0 nO nH nN nn n0 nA n0 f A o n n n 0 A A r '9 A O H f )A A A A A c* o o o o A m X i a 023(91: quantlafcad and printad b y hoj 5/28/99 Q uantify C alib ratio n Raport to*120, r t l C a l ib r a tio n : C:\9AMLTWC\rata2.VK3\CuxvaDB\0S2599a L a a t a o d i f i a d : Wad a y 2 0 7 :5 9 :3 9 1999 V rintad: Wad a y 2 0 1 :2 1 :0 3 1299 Van l 000703 Q uantify C alib ratio n (a p a rt toxl20, r t t c a l ib r a tio n ! C:\MM9LTWC\rate2.P9O\CurraD9\052399a L a a t a o d i f l a d : Wad May 2 0 7 :5 1 :3 1 P rinted: Wad May 29 0 9 :2 1 :0 9 1 Pago 2 alia 09249! q u an tlated and p rin ted by boj 9/29/99 000704 Q uantify C alib ratio n ta p o rt toxl20, r t l C a lib ra tio n s C:\M M SU N C\rata2.m o\CurvaD B\052599a L a a t a o d l f l a d : Wad May 2 0 7 s S (:3 S 1999 V rlntads Wad May 2 0 9 :2 1 :0 5 1999 000705 Q uantity C alibration Hapert toxi20, r t l Calibration* C: \M*4IL.nOC\rata2.P*O\CoxvDB\0S2S99a Laat modified: ad May 2 07:91*39 1999 Vrintad* ad May 2 09:21:09 1999 a lia 092496* quantin te d and p rln ta d by bo j 9/24/99 000706 Q uantify C alib ra tio n K apert to*120, r t l Calibration: C:\HASaLnoC\rats2.FKO\CarvaOB\032399a Laat modified: Wed May 2 07:55:3 U M Printed: Wad May 2C 09:21:05 U M Fan a Amalia 062498 : q u a n tla ta d and p r in te d b y h e] 5 /2 6 /9 9 000707 Hathod Report Method til: Last modified: Compound: Printed: C:\HASSLWOC\rats2.PRO\MathDB\OS2599a.mdb Wad Kay 2 07:18:17 19990 1: P O M Compound H u n Internal Rot.: Quantity Tracai Cane, of Standard*: Usar RF Value: Usar peak Factor: Integrata Window Factor: Peak Location Retention Time (mina): Relative Retention Tima: Tima Window (mina): Peak Selection: Response Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Concentration Obits: Noise Peak-to-peak amplitude: Smooth Smoothing: Window is (scans): Number ot smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: Peek Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative area: Absolute area: PCM [Hono] TIC Cone. A 1.000000, Disabled 1.000000 2.000 5.010, Enabled 0.000, Disabled 0.304 Nearest External Areas Linear Exclude 1/X None (0 'D i s a b l e d 3 2 30.00 70.00 4.00 10.00 Disabled 10.00 50.00,* Enabled 0.00, Disabled , 3.00, Enabled 0.00, Disabled - l a c o s / u l n _______________ Page 1 000708 Hathod K aport Hathod fila: Last modified: C:\HU3LnK\rats2.MO\XathDB\052599a.ndb Mad Hay 26 07:11:19 19990 Compound: 2 : H513 P rinted: Mad Hay 2 0 1 :2 1 :1 9 1999 A hJ i * Compound Nana: Internal Rtf.: Quantify Traca: Cone* of Stmndarda: Uaar RT Value: User Peak rector: Integrate Nindow rector: Peak Location K513 (None) TIC Cone. A 1.000000, Disabled 1.000000 2.000 Retention Tima (mine): Relative Retention Tima: Time Nindov (mins): Paak Selection: Resnonse 5.531, Enabled 0.000, Disabled 0.233 Nearest Response Type: Response: Calibration Curvea External Areas Polynomial Type: Point of Origin: Fit Weighting: Axis Tranefornation: Concentration Linear Exclude . 1J * Mona Units: Noise Feak-to-peak amplitude: Smooth 64 Smoothing: Window alza (acea): Number of smooths: Smoothing method: Baaellnea Disabled 3 2 Join valley threshold: Reduce peak tailing: * Raise baseline maximum: Peak SeDaratlon 30.00 70.00 4.00 Draw vertical threshold: Detect shoulders: Shoulder threshold: Response Threshold 10.00 Disabled io.oo Relative height: Absoluta height: Relative area: Absolute area: 50.00 Enabled 0.00 Disabled 3.00, Enabled 0.00, Disabled ___o l m I i Uc o r h J il Paja 2 000709 Method Report Method file: Last modified: Compound: Printed: C:\MAS3URM\rats2 .PR0\KetbDB\0S2599a .mdb Nad May 26 01:10:1? 1999a 3: M613 Ned May 26 00:21:19 1999 ^ mfh Compound Nana: Internal Ref.: Quantify Trace: Cone, of Standards I M13 (Nona) txc Cone. A Ueer RT Valus: Osar Peek Factor: Integrata Window Factor: 1.000000, Disabled 1.000000 2.000 Fasi: location Retention Tina (Bins): Relativa Retention Tina: Tina window- (nine): 5.001, Enabled 0.000, Disabled 0.210 Peak selection: Response Nearest Response Type: Response: External Areas Calibration Curves Polynomial Type: Point of Origin: n t Weighting: Axis Transformation: Linear Exclude 1/X Nona Concentration Units: Noise Feak-ta-peak amplitude: 19 Smooth Smoothing: Window also (scans): Number of smooths: Smoothing mathod: D i s a b l e d 3 2 Baselines Join vallay threshold: Reduce peak tailing: Raise baseline maxima: 30.00 70.00 4.00 Peak Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: 10.00 Disabled 10.00 Response Threshold ' Relative height: Absolute height: Relative area: Absolute area: 30.00, Enabled 0.00, Disabled 3.00, Enabled ' 0.00, Disabled OLIWS (AC Ofhufa,? Page 3 000710 ltethod Report Method m * i Lilt modified: Compound: P rinted: CI \MA3SLYNX\xats2.PRO\M*tMJB\OS2599a.ndb ad May 28 07:18:17 1 9 9 4: Pros Wad K ay 28 0 8 :2 1 :1 9 1999 Compound Mao: I n t a n a i Raf.: Quantify Trac*: Cane, of Standard*: Osar RT Valua: Usar P*ak Factor: Zntsgrata Window factor: Peak Location Retention Tin* Inina): Salativ* Retention Tina: Tin* window Inins): Peak Salactlon: Raapons Response Typa: Rasponsa: Calibration Curves Polynonial Typa: Paint o Origin: Fit Weighting: Axis Transformation: concentration Unita: Kola Peak-to-paak enplltude: Snooth Smoothing: window six (scans)t Humber of smoothes Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Rais* baseline naxinun: Peak Saoaration Draw vertical threahold: Detect shoulders: Shoulder threshold: Rasoona* Threahold ' Relative height: Absolute height: Relative area: Absolute area: pros (Hone] TIC Cone. A 1.000000. Disabled 1.00Q000 2.000 5.281, Enabled 0.000, Disabled 6*2*3 Nearest External Areas Linear Exclude 1J X Hone 72 .Disabled 3 2 30.00 70.00 4.00 10.00 Disabled 10.00 SO.00, Enabled 0.00, Disabled 3.00, Enabled * 0.00, Disabled A h ,,L L2HW IA t os/ z U m Pig* 4 000711 Method R eport Method tilo: Last modified: Compound : i r l a tadi C:\MM3LYNX\rata2.PRO\KathDB\052399a.ndb Mod May 26 07:19:17 19990 5: IS a d May 26 0 9 :2 1 :1 9 1999 Compound Nan: Internal Rtf.: Quantify Traca: Cone, of Standards: User nr Vala: Osar Paat Tactor: Integrate Window Factor: Peak Location Retention Time (mina): Relative Retention Time: Time Nindow (mins) Peak Selection: Response Response Type: Rasponee: Calibration Curvea Polynomial Type: Point of Origin: rit Weighting: Rucia Transformation: Concentration Units: Kola Peak-to-paak amplitude: Smooth Smoothing: Nindow tilt (scans): Number ot 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 (None) TIC Fixed 1.000000, Disabled 1.000000 2.000 5.029, Enabled 0.000, Disabled 0.304 Nearest External Areas . Linear Exclude 1/X Mon. 93 .Disabled 3 2 30.00 70.00 4.00 10.00 Disabled 10.00 30.00, Enabled 0.00, Disabled 3.00, Enabled 0.00, Disabled 4 / J f t O U W _____ l A c Pag* s 't r 000712 ^W/An_______________ M asslynx - Sam ple L ist Sample L is t C:\M ASSLYNX\rats2.PRO\Sam pleDB\060199c.SPL Printed: Tue Jun 0116:19 :1 8 1 9 9 9 F ile Nam e 1 060199020 2 060199021 3 060199022 4 060199023 5 060199024 6 060199025 7 060199026 8 060199027 9 060199028 10 060199029 11 060199030 12 060199031 13 060199032 14 060199033 15 060199034 18 060199035 17 060199036 18 060199037 19 060199038 20 060199039 21 060199040 22 060199041 23 060199042 24 060199043 25 060199044 26 060199045 27 060199046 28 060199047 29 060199048 30 060199049 31 060199050 32 060199051 33 060199052 34 060199053 35 . 060199054 36 060199055 37 060199056 38 060199057 39 060199058 40 060199059 41 060199060 42 060199061 43 060199062 44 060199063 45 060199064 46 060199065 47 060199066 48 060199067 49 060199068 50 06019906S 51 060199070 52 060199071 53 060199072 54 060199073 55 060199074 56 060199075 57 060199076 58 060199077 59 060199078 60 060199079 ' File Text methanol blank methanol blank tox120, rbl04199-wblk-2 tox120, rbl04199-lblk-2 tox120, rbl04199-5 ppb-2 tox120, rbl04199-10 ppb-2 tox120, rbl04199-25 ppb-2 tox120, rbl04199-50 ppb-2 tox120, rbl04199-100 ppb-2 tox120, rt>l04199-250 ppb-2 tox120, rbl04199-500 ppb-2 tox120,rbl04199-750 ppb-2 tox120, rbl04199-1000 ppb-2 methanol blank to x120,1M -g 1,4/19/99 to x120,2M -g 1,4/19/99 to x120,3M -g 1,4/19/99 to x120,4M -g 1,4/19/99 tox120,5M -g1t 4/19/99 tox120, rbl04199-250 ppb-co-1 methanol blank to x120,6M -g 1,4/19/99 to x120,7M -g 1,4/19/99 to x120,8M -g 1,4/19/99 to x120,9M -g 1,4/19/99 to x120,10M -g 1,4/19/99 tox120, rbl04199-250 p pb-cc-2,5/28/99 methanol blank to x120,11M -g 1,4/19/99 to x120,13M -g 1,4/19/99 to x120,14M -g 1,4/19/99 to x120,15M -g 1,4/19/99 tox120, rbl04199-250 ppb-cc-3 methanol blank tox120,6M -g1, ms, 4/19/99 tox120,6M -g1, msd, 4/19/99 tox120,13M -g1, ms. 4/19/99 tox120,13M -g1, msd, 4/19/99 tox120, rbl04199-250 ppb-cc-4 methanol blank tox120.3M -g1.m s. 4/19/99 tox120,3M -g1, msd. 4/19/99 to x120,41M -g 3.4/19/99, d10 to x120,23M -g 2,4/19/99 to x120,24M -g 2,4/19/99 tox120, rbl04199-250 ppb-cc-5 methanol blank to x120.25M -g 2,4/19/99 to x120,26M -g 2,4/19/99 to x120,27M -g 2,4/19/99 to x120,29M -g 2,4/19/99 to x120,30M -g 2,4/19/99 tox120, rbl04199-250 ppb-cc-6 methanol blank to x120,31M -g 2,4/19/99 to x120,33M -g 3,4/19/99 to x120,34M -g 3,4/19/99 to x120,35M -g 3,4/19/99 to x120,36M -g 3.4/19/99 tox120, rbl04199-250 ppb-cc-1 Page 1 MS File 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9MIN-PO AA-513-613 9M IN-POAA-513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9MIN-PO AA-513-613 9M IN-POAA-513-613 9M IN-PO AA-513-613 9MIN-PO AA-513-613 9M IN-POAA-513-613 9M IN-PO AA -513-613 9MIN-PO AA-513-613 9M IN-PO AA-513-613 9MIN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M 1N -P O A A -513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-POAA-513-613 9M IN-POAA-513-613 9M IN-PO AA-513-613 9M IN -P O M -513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 v 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-POAA-513-613 9M IN-POAA-513-613 9M IN-POAA-513-613 9M IN-POAA-513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9 M IN -P O A A -513 -6 1 3 9M IN-POAA-513-613 9M 1N -P O A A -513-613 9M IN-POAA-513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-POAA-513-613 9M IN-PO AA-513-613 9M IN-POAA-513-613 9M IN-POAA-513-613 000713 In let File 9m in-2 9m ln-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m ln-2 9m ln-2 9m in-2 . 9min-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m ln-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m ln-2 9m ln-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m ln-2 9m in-2 9m in-2 9m in-2 9m ln-2 9m ln-2 9m ln-2 9m ln-2 9m in-2 9m in-2 9m in-2 9m ln-2 9m in-2 9m ln-2 9m in-2 9m ln-2 9m ln-2 9m in-2 9m in-2 9m ln-2 9m ln-2 Masslynx Sample List Sam ple L is t C :\M ASSLYN X\rats2PRO \Sam pleDB \060199C.SPL Printed: Tue Jun 01 16:19:181999 F ile Nam e 61 060199080 62 060199081 63 060199082 64 060199083 65 060199084 66 060199085 67 060199086 68 060199087 69 060199088 70 060199089 71 060199090 72 060199091 73 060199092 74 060199093 75 060199094 76 060199095 77 060199096 78 060199097 79 060199098 80 060199099 81 060199100 82 060199101 83 060199102 84 060199103 85 060199104 86 060199105 H ie Text methanol blank to x 1 2 0 ,3 7 M -g 3 ,4/19/99 to x 1 2 0 ,3 8 M -g 3 ,4/19/99 to x12 0 ,3 9 M -g 3 ,4/19/99 to x 1 2 0 ,4 0 M -g 3 ,4/19/99 to x 1 2 0 ,41 M -g 3 .4/19/99 tox120, rbl04199-250 ppb-cc-2 methanol blank to x12 0 ,4 2 M -g 3 ,4/19/99 to x 1 2 0 .43M -g 3.4/19/99 to x 1 2 0 .45M -g 3,4/19/99 to x 1 2 0 ,4 6 M -g 3 ,4/19/99 to x 1 2 0 ,4 7 M -g 3 ,4/19/99 tox120, rbl04199-250 ppb-cc-3 methanol blank tox120, rbl04199-wblk-2 tox120, rbl04199-lblk-2 tox120, rbl04199-5 ppb-2 tox120, rbl04199-10ppb-2 tox120, rbl04199-25 ppb-2 tox120, rb!04199-50 ppb-2 tox120, rbl04199-100 ppb-2 to x l2 0 , rbl04199-250 ppb-2 tox120, rbl04199-500 ppb-2 tox120, rbl04199-750 ppb-2 tox120, rb!04199-1000 ppb-2 Page 2 M S F ile 9M IN-PO AA -513-613 9M 1N -P O A A -513-613 9M IN-PO AA-513-613 9M IN-PO AA -513-613 9M IN-PO AA -513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-PQ AA-513-613 9M IN-PO AA -513-613 9M IN-PO AA-513-613 9M 1N -P O A A -513-613 9M IN-PO AA-513-613 9M IN-PO AA -513-613 9M IN-PO AA-513-613 9M IN-PO AA -513-813 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M 1N -P O A A -513 -6 1 3 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-PO AA -513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 9M IN-PO AA-513-613 Inlet File 9m in-2 9m in-2 9min-2 9min-2 9min-2 9m in-2 9min-2 9min-2 9m in-2 9m in-2 9m ln-2 9min-2 9m in-2. 9m ln-2 9min-2 9min-2 9min-2 9m in-2 9m in-2 9min-2 9m in-2 9min-2 9m in-2 9min-2 9m in-2 9m in-2 000714 jp ^ > I 6 _________________ __________________ S can n in g Method R aport Method: C:\MRSSUrMX\MTS2.9N0\ACSaDB\9KZN-9CM-S13-13 ' Last Modified: Toa Jun 01 14:34:0 19 Prlntad: tua Jun 01 16:19:2 199 S o lv en t D alay | a ln a ) : 0 .0 0 Tunotion : 1 M M of 1 Maaa air ( 199- > Istar Channel Balay ( Saca ) : 0.03 Span ( Daltons ) > 0.00 Start Tina ( Mins ) : .0.00 End Tina ( Mina ) t 9.00 Repasts : 1 Channel Tarant Daughter Dwell (Sacs) Coll Energy (aV) Cone ( V > 1 ' 413.00 169.00 0.30 20 13 :lunation 2 M M of 1 Maas Vais ciw- ) ( )Inter Channal Dalay Seca ( )Span Daltons i )Start Tina 1 Mina i ( ) :End Tine Mins :R e p a s t a i Channal Parent Daughter 0 a03 0.00 a0.00 9 00 1 Dm U . (Sees) Coll Energy (aV) 1 513.00 169.00 0.30 20 . (Coo V 1 15 lunation : 3 Mm of 1 Mean M r (CSV- ) ( ) :Inter Channel Dalay < )Span Daltons i ( ) :Start Tina Mina { ) :End Tina Mins :R a p a a t a Sacs Channal Parent Daughtar 0.03 0.00 0.00 0.00 1 Dwell (Sees) Coll Energy (eVl <Con V 1 1 613.00 169.00 0.30 20 15 Tunction : 4 M I of 1 Mesa 9alr ( 189- > lutar Channal Dalay ( Seca ) 0.03 Span ( Daltons ) : 0.00 Start Tina ( Mina ) : 0.00 End Tina ( Mina ) : Repaata : 9.00 1 Channal Parant Daughtar Duali (Seca) Coll Energy (eV) Cona ( V ) 1 427.00 60.00 0.30 40 .60 Page X 000715 1 (o ltfe a Tuning Method Report Method: C :\MASSLXNX\RATS2. PRD\ACQUDB\PFOS Printed: Tue Jun 01 16:20:59 1999 Page 1 1 SOURCE ( ESP- ) j Capillary Cone Extractor RF Lens J Source Block Temp. J Desolvation Temp. ]1 . Pressures 1 Analyser Vacuum 1 | Gas Cell \ | i i Set Rdbk 3.00 2.97 15 '-14 50 0.2 150 152 250 253 Rdbk 1.6e-4 5.1e-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier Set Rdbk 15.0 1 5 . 0,, 2.0 * . 0.0 56 650 MS2 LM Resolution HM Resolution Collision Ion Energy Ion Ener g y 'Ramp Lens 8 Lens 9 Multiplier Set Rdbk 15.0 15.0 20 2.0 0.0 40 0 650 21 38 20 000716 FACT: DATA REVIEW SUMMARY FORM f aOste: Analyst: FACT Study Number Matrix Time Foists /o k ite ) ?TL Dilutions? A s' Analyte 1: A h A /f' W a r R ange: / ~ ////// _ LOQ br ds data se t Reevaluated fir differentrange? a/ \JAnalyte 4: Acceptable Linear Range: LQQ for dus data set iluated for different range? Analyteo: Linear Range: LOQ for thu data set Re-evaluatedfix dif ferent range? Analyte 2: s h ir t Acceptable T,mear Rang - /////^ LOQ for this data se t S S ^ -G /Y S Re-evaluated for different range? J Analyte 3: A lt/? Acceptable T.nearRange: fj T f LOQ for ds data set ST*C A A Re-evaluated fix differentrange? Analyte 6: \ Acceptable Linear Rail<Mk* LOQ fix ds data sett^ Rc-cvaluatedfor diffoMotrange? \ Analyte 7: Acceptable linear Range: LOQ for ds data set Re-evaluated for different range?' 000717 \ t t / t O / Coti A q p 3 U T i t l p u * p a 7 3 u * n b : 6 H J 0 * t t W a> in i> g h o v g uj*-gu w4 gH<oii**0gi<0iiauii0Aiw0iM0tHi0uiaigii0tuifuu*MuiiN<iHiOt0^ a g oHo0 HIooO*Uoo>(HooAH1oo0HIooOtHot>Ool.0OlgOo_0OaltOo0tOill00OoO0VVOoAIOt00QUo*OW0MOQO)(H00OOlOo0WOO<<oI0OAO0oWlO0OogI4O0O|Oo(OO0i0oO|Ot00o0O|lO00o*IO|OA0Uo|OOt0M0o|OalOH00oO00So00(OOo(0o40O01o*o0J oK(go0*oI(o0-W>I (oo*o04*(ooMo0Wo1o-e004NoNo1oMO0MooVo1JA0 ooOV(o40Ao0oV((o00Ooo0V(o0OooVVo4OOooV0oVPOooUtVoo0o*tvooHoaUoMtoiooooAo1O0*A1oVtoOA^SoVVo0UODIVo1Vo0oVO0OotoAA(oRoO oi0otoonto0otoooo0outo(0oto0o1to*o0o0oVteuUoOoNo0uoVto*Oo-ou0ottooo0ooto0oAoVtooOoAoVo(O0c0oSOP-0-oOt(o0-0v(-oO0o0-t0O-oOtotO-0toO0V-0oOOt-0V-0ooOt-Oo-0tootO00V0-ooOv-000-(SoOOt-00O-ooOi-0V0-oo0Ot-0V0-ooOOv00-too0OtoV0-oovO-001o-ooO0-vV0-oopO0-tIVoo-oOtOo-oVo-OvOoo-oO(t-0ooVoOto0ootOtOo~ovoO-O0o-oOVt-oo0-oOVtoo^DoOt"o(o0otOto~0ovVoOK_o0x" XKXKXXX XXXX!J*KXX S 5 XXXXXrtXXXXrliH-OTnXO(XOtfXtOiXrOrXtO|XVfo o#* ort rot oct ort oft o? o n rt rt OOo rtitrt ooo XXX . . f t IT ItltftlT s......s.........X X X V0r trOtxrOtxOf xt Orxt OrxtOxr trOBrOf xtOrxtOrxtOxn Onx Orxt o oo ___ 9oooooo gooooo>.0 0(0K 0i M30 0M 0N <( H W H NXM 3000 0 MKIMMNM 09 N0 0N 0N 0N 0N 0N 3a*0M 0M 0M 0M 0N 0M v- **u M M 3**** M I M0 0M 0MM0NM0NM30 K IN N OOO O ' *> o * n n n n r t n l n r r tr t n r t r r t r r r r rTrh Sxx km S h x h Sf h VT K h X m >0 0 0 0 0 * 0 0 iX X X X X n n l - ST a r f l g 0 0 0 0 0 0 9 0M 0N 0N M0 0N 0N O8oM0M0 . . . . __XXX *&SS!ae r t x t r t r t r t r t r n0J rtrtr -4c <r 3- i P T o o o o o o o (-HX OOOOXOt I I ( I 0 0 05 a ^,(1 U N N M N N N N * U U ftH H A N SSxxS epX o* M 0i W 0i U 0i U 0i U 0T N " *1` * X M0 N N MV N M* X HVO * - O J (00 H1*0 0NV 0H *H**M -09 **0* 0*1 0*. 0. 0. * h X9 hX I *O 00H I 0H I 0H 0" XV- H * * 3X *M -*** Xn i . -I 0 rtrc rcrcT it >*>->->- 0 0 0 0 0 0 0 OO0 0 0 vo vo **VO-**to-3X8x1IHt Ii IIIIII H JU N W U N mi s i , 0ooooO l D O K O O t t W * N 'S*'S. V* N10.(0SVNON(0 s 0 VO VOVO0 to to ve ?0 0 * 0 0 N \SSS\ OV0V0 e v o o sss 7 TM So N* S* S* *S U o HV0 HHHH va to vo vo V0 vo . . . e e N V .V S S S NNNNfk* Otovo1010V0u h h h h h \t s \s UHHHV O NVONOSV00 S0 to V0 V0 V0 vo vo vo to to vo >V0 VAM V0 * s S ill! u& * I**** NSSSN U M - *- M o vo vo 0 vo _ sw s. S vo vo vo vo 7vo VOVOVOlO ***0 inm toto to vo O 0S S W ,, *s.(OV0 vo vo V VOVOV0 (O 10 u__*__*__*____*_? f I I I I I I NvtHoHvoMvoMvoHo HO i4n Uo Ne Ho Uo teN oH U t IO O ttWoo v(oONtvooVvvooSvvoo 0" 0 O O O S HM XX - 8 S S 3 7 MM dt^ dt A A A M 1 MMNM 3? >iUI s? 15 M It f s si ; V AM * ft & i" ca e- !r f . a o o o P 05 HAUM H N U U 4H U M H H U 0 O 0 l* 0 M U U U U U U U l U U t f U .l*inUiVMOUMnOUI4O(0M|*(|l(OUMO(MllU(O(fMlllMO<n NO4 UMO NMO|*O*NO| MO* **O N0O U0O4*O0 0O4 o*U Oo* Hou Ao* Uob o* peMo*Uou*o*4 o*0 o*U oo0 oA to* foN 4oH 0o* Hou 4o*Oo*HoM0onH oo| o*l oNV o** 1*10 tniAtnlnintnininmui 0U 0W vo** NOvo *Ovo UOK**O100M4 UON UOA UOO OuC JO0* 0* 0uU u001 uu*u*uu*u 0N0 U*U U*0 *0X 0 *0U O0O O4U UMO 10 (1* u * u u u u u u u * u * u 0u0 VpOvMo O VO HOU 40 nUOuUOoNOu UO4 MO0 *NO u*O iNUNUO*40u **i i* a s UM** *(*IP *N U Mn h *t*04UNOeO NU0U HOV0UI00 HI tJ M in * U * O V 0 M O U H luUno4UunPot0h0uNm*m4n40o(< i a * H to M m ^ M vo i0 (* N U i4 * a K t* u o a ve a to to u* a w est O 4U M H M U 4 VIU00 * u n U 0 0 N N 4 0 O 4 UO o o n 0 O O O o v 0M(n * H 0OO 0UON*N 4N4IAN*mH- uwoienun it MMOWOV0 MOvOtOMOMMMnMnOOMMWOOOU A n A U t t S e U 0 g u O e * S A A N O U * 4 l0* A M O r ` A O * * 0 *M *W U *n A U M N U > U U H M H 0 M4O H H U AA 4 U * 4 * A U * n 4 A 4 4 4 U N U e A O U A M 4 l0 U * ggggggggggggggggggggggggig$ M VOM An M M W M U M M 0 4 O 4 A A NV0 N * U * H 4 H H O * 0 OOVS uuMotovooMMmuvo U(H0 4 N U 0 B * 0 A ssm sssm s N to * 0 00 00 gg JI0 W O U 0 0 A * HM h OMO U N A U A O 4W0 4 U M N A 0 * O 0 U U 4 OO 0M u 0 0 M 00 01 U 10 ? g UMMH U O O N 0N U HH U W H O U *U 4 *(0 I0 N V * U 0M AABH *N H O A H 0 |0U 0 A M W * O H 0 4 U U A B U N 4N U 0 HOW4 A A A H A M O A O gggggggg%S$gg r .- o00* cr * T AI l0 * H M MM 4MOON0 I HANHn O0V00U4U0 I Q u a n tify Compound Summary l U p o r t to*120, 1*3# r t l ampio tlat: C:\MMSLYMX\rits2.mO\SamplaCa\0CO199e Laat modlfiod: Tuo Jun 01 16:18:01 i m Hothod : Ci \MAA5LYHX\rats2.9N0\HmthD\040199e Laat modlfiod: Nod Jun 02 06:48:03 199 Job Codo: frintod: Nod Jun 02 07:20:4? 1999 Compound 2: HS13 Hama 1 040199020 2 040199021 3 04Q199Q22 4 040199023 3 040199024 4 040199Q25 7 040199024 8 040199027 $ 040199028 10 040199029 u 040199030 12 040199031 13 040199032 14 040199Q33 IS 040199034 14 040199035 17 040199034 18 040199037 19 040199038 20 040199039 21 040199040 22 040199Q41 23 040199042 24 040199043 2S 060199044 24 040199045 27 040199044 28 040199047 29 040199044 30 060199049 31 040199Q5Q 32 040199051 33 060199052 34 060199053 35 040199054 34 040199QS5 37 040199054 38 040199057 39 040199054 40 060199059 41 040199060 42 040199061 43 040199042 44 040199043 45 040199044 44 040199065 47 040199064 48 040199047 49 040199044 50 040199049 51 060199070 52 060199071 S3 060199072 54 060199073 55 060199074 54 060199075 57 060199076 58 060199077 59 060199078 40 060199079 41 060199080 42 060199081 43 060199082 44 060199083 45 060199084 44 060199085 47 060199086 48 060199087 89 060199088 70 060199089 71 060199090 72 060199091 73 060199092 74 040199093 75 060199094 74 060199095 77 060199094 78 060199097 79 060199099' 80 060199099 81 060199100 82 080199101 83 060199102 84 060199103 85 060199104 84 060199105 Taxt nathanol blank nathanol blank tox!20, rbl04199-nblk-2 toxllO, rbl94199-lblk-2 toxl20, rbl04199-S ppb-2 (0X129, rb!04199-10 ppb-2 toxUO, rbl04199-2S ppb-2 tOX120, rbl04199-S0 ppb-2 toxl20, rbl0419-100 ppb-2 toxl20, rb!04199-2S0 ppb-2 (OX120, rbl04199-500 ppb-2 (OX120, rbl04199-OSO ppb-2 (OX120. xbl04199-- 1000 ppb-2 M(hanol blank (OX120, IH-gl, 4/19/99 (OX120. 2H-gl, 4/19/99 (OX120, 3M-gl, 4/19/99 (OX120, 4H-91, 4/19/99 (OX120, SK-ol, 4/19/99 (OX120, rbl04199-2S0 ppb-ce-1 m(hanol blank (OX120, CK-fl, 4/19/99 (OX120, TK-ol, 4/19/99 (OX120, OM-gl, 4/19/99 (OX120, SK-gl. 4/19/99 (OX120, lOK-gl, 4/19/99 (OX120, zbl04199-2S0 ppb-ec-2, rn.th.nol blank (0X120, llH-gl, 4/19/99 (OX120, 13M-gl, 4/19/99 (OX120, 14M-91, 4/19/99 (OX120, 1SK-ol, 4/19/99 (OX120, rbl04199-250 ppb-cc-3 xa(hanol blank toxl20, CM-gl, , 4/19/99 (OX120, K-gl, msd, 4/19/99 toxl20. 13H-gl, na, 4/19/99 (OX120, 13H-gl, nad, 4/19/99 (OX120, rbl04199-250 ppb-cc-4 nathanol blank (OX120, 3M-gl, ns, 4/19/99 (OX120, 3K-gi, nod, 4/19/99 (OX120, 41M-g3, 4/19/99. dlO (OX120, 23K-g2, 4/19/99 (OX120, 24M-g2, 4/19/99 (OX120, cbl04199-- 230 ppb-ce-5 nathanol blank (OX120, 25M-g2, 4/19/99 (OX120, 2<M-g2, 4/19/99 (OX120, 27M-g2. 4/19/99 (oxl20i 29M-g2, 4/19/99 (0x120, 30M-g2, 4/19/99 (OX120, tbl04199-2SO ppb-cc-4 nathanol blank toxlOO, 31M-g2, 4/19/99 boxl20, 33M-g3, 4/19/99 (0x120, 34M-gl, 4/19/99 (OX120, 3SH-g3, 4/19/99 (oxUO, 3<M-gl, 4/19/99 (oxl20, kbl04199-230 ppb-cc-1 na(hanol blank (oxUO, 3m-gl, 4/19/99 (0x120, lK-gl, 4/19/99 (0x120, 39K-g3, 4/19/99 (OX120, 40M-g3, 4/19/99 (OX120, 41M-g3, 4/19/99 (0x120, cbl04199-23O ppb-ee-2 nathanol blank (OX120, 42M-gl, 4/19/99 (OX120, 43K-g3, 4/19/99 (OX120, 43H-gl, 4/19/99 (0x120, 4SM-g3, 4/19/99 (OX120, 47M-g3, 4/19/99 toxl20, rbl04199-230 ppb-cc-1 nathanol blank (OX120, xbl04199-wblk-2 toxl20, rbl04199-lblk-2 (OX120, rblO.lSS-- 3 ppb-2 (0X120, rbl04199-10 ppb-2 toxl20. tbl04199-23 ppb-2 (OX120, rb!04199-30 ppb-2 (0x120, rbl04199-100 ppb-2 (0x120, rbl04199-2S0 ppb-2 tox!20, rbl04199-300 ppb-2 COX120, rbl04199-130 ppb-2 tox!20. rb!04199-1000 ppb-2 S/20/99 Amnlla 042491: q u a n tia to d and p rin to d b y b o j 4 /0 2 /9 9 a 2 *> Analyta td Cono Analyta Analyta Analyta Standard 5.5 Standard 11.10 Standard 27.10 Standard SS.SO Standard 111.00 Standard 270.00 Standard 55.00 Standard 033.00 Standard 1111.00 Analyta Analyta Analyta Analyta Analyta Analyta QC 270.00 Analyta Analyta Analyta Analyta Analyta Analyta OC Analyta 270.00 Analyta Analyta Analyta Analyta QC Analyta 271.00 Analyta Analyta Analyta Analyta QC 270.00 Analyta . Analyta Analyta Analyta Analyta Analyta QC 27.00 Analyta Analyta Analyta Analyta Analyta Analyta QC 270.00 Analyta Analyta Analyta Analyta Analyta Analyta QC 278.00 Analyta Analyta Analyta Analyta Analyta Analyta QC 270.00 Analyta Analyta Analyta Analyta Analyta Analyta QC 270.00 Analyta Analyta Analyta Standard S.S Standard 11.10 Standard 27.00 Standard 35.(0 . Standard 111.00 Standard 271.00 Standard 55.00 Standard 133.00 Standard 1111.00 ST S.310 S.484 3.477 3.43 3.470 3.437 3.457 3.481 5.47 5.413 3.474 5.4 5.477 5.509 3.4(1 3.473 S.S03 3.470 3.479 3.482 3.492 3.491 5.4(0 3.473 3.430 3.4 3.487 3.474 3.305 3.475 3.490 5.47 5.474 3.412 5.300 3.490 3.474 5.4(3 5.4 3.47 3.479 5.49 5.4(0 5.4(3 5.493 5.514 5.437 5.49 5.492 3.494 3.472 3.473 At m 6 Cone, fina %0v 33.86 bb 4 38.43 bb 17 155.79 bb 33 340.82 KK 58 626.52 bb 78 650.34 KM 105 1156.36 KK -31 40 23 13 2 4 22 215.92 MM -22 28 286.55 MK 3 26 259.87 M M -7 24 238.96 bb 29 292.29 M M 22 215.83 M K 26 265.21 MM 29 295.89 MK 6 23 224.10 MM 23 225.97 bb 10 78.75 bb 115 1272.23 M K 147 1632.39 MM 27 271.64 MM -2 99 1083.93 M M 123 1360.34 MM 191 2126.03 M M 118 1302.00 MM 75 920.19 MM 25 250.88 bb ,7 -10 87 956.99 MK 102 1127.3? M M ` 135 1492.73 H i 92 1013.14 MM 92 1010.59 Ml 26 260.57 bb -6 100 1104.83 Ml 75 819.95 Ml 109 1201.84 MM 96 1051.95 W 86 942.87 MK 29 294.92 bb 6 78 851.36 MK 97 1067.95 MM 57 610.50 Mf 65 707.74 bb 47 496.73 bb 30 307.89 bb 11 4 14.64 MK 6 40.05 MM 10 1.11 bb 25 254.54 MM 46 490.00 MM 78 854.07 MM 91 995.71 M M 32 -29 -27 -6 -12 3 -10 000719 SS2SS2Sii3i!iCrfiiSS5S3SSSSiSSSSi52SSSSSil:fiSCi:i:SSSt5SSS:!SiS!gS5iiS!tiS!5iiSS = iJS:S5:UEiS--ui*.u-- 22222222222222222222SSS22SSS22SSf2S2SS2S2f22SSS2S2S2SSSS222SS2S2S22gg|25|!2222gg| T S ooooqqooS ooooooooooooooooooooooeoooooooooooooooog iaaa*a ...........Hoooooooooooooooo^eooooooodooooodooovo ot oAoUoMo HM >etfio0 *i suwi*ADUi N0 WHUOM0A <a aJiniuait *a iwaMAH(Oi t( tt 4**lJ A'>J('i4*^'UiM'4H>4o-i> <o'aJ*n AJAAO iUoit OSO luOOMOiHOO OOI Oe o Ao"OUfUOtUOUUOO*OOUOONUOH>OOUtOUSiOV*Og*aO*UO*lO**OU*MO*HO*OO* WOa U*OVJO)AOUO UO WO0_..WU...O_.0.W_N.._..O._UH0.._.._U0o__N<_0_aN_0_N_0_wN_a0_M_i_0_iM_0a_Nx0Muv0NoM0Kt a0 NO . !ei SS e rtrtrtE S aoooooog m i Sa* OBOI KXX) Io o o o o o CX X X X X X OOOOOO t t #r r t t r t r t rtiti OOOOOO O O O O O O OOP M X X X X X - X X X X X X rt X X X hhhmhh M M M M M M ?... 9 O 0-0 O O O g.oio o o o o : fftittffrtrt OOO o o o o p * X X X t* X X X X X 1 M M M N N X n a rt o XX m t rr tr r t rt ooooo XX XX XX XX XX s xmnwm ffr tttffr tl rtrtrtitrt XnOX XnOX Xm-t<I>0H"xNH0x"Nr*"fIt0H'Nx'0H"Nx0HM"x0HMx" 0HxN" B.'" it or t or t ? o o ? S X X X X X X rt MMNMNM >g O O O O O O 9 O O O O O O --------------->009o O *O *O O* O r t r t r t rt c " o o oc X X rtX> V MNMWNM i Nf o o o o o o 9 OC O' " tf*rtffr*r*rfnrfW I I O O O O O O O p i I X K X X X X X X rt rt l SrT IMMNMMNMNt H >0 0 s0 0 0 *0 0 0 9o 9O t* * *- m HAAUUO N u u UUU H UMMMM i oooooooooooa s s s s s s a : s s s -- **-------O oxoi I IIOTAA4I OAAi S E i S K a S . 0 1 1 1 1 7 1 0 1 tm * *irHr * H <HHHHHHV^, WUUUW 9 XAOOOO (THUUWUW l OOO w Ir 1*n0Au u%Uv s c iis iia a s tot I 0 0 9 > A 4 4 HH KrtKiNU* 0 *AA l ____- O O O X ithhX HA` HK) H 4K` H<` 9 O O......H......H......H......H.... 0 0 * * * o* " ?I 8 f <l*iltio *f* * * * * > s. s. sT * * * * * ? * 1 1 e e *t* 3 OOO w I I l 1 I I I I I ( uo> ae MH OO UlMHtfH O 4* 0 _ O* S' a Hi- & INN M S\SV \ OOOOOO N V N SS OOOOO OOOOO N SW SS oI DoHoHoHoMoH N \> \\ *0 O O O O O *0 O O O O O N SN S n\SV 000 N S N 'V N. S Wo oHoHoH oH oH N SSSN 00000 OOOOO eb N N SV i* O Os O\ Os * s* EE a * 0. o* M SSSS ItHHHH OOOOO SSSN V Oo o o ^ow M'.. U>H HH O O H tOt o ia ssss *>.0000 "> 0 0 0 0 5 . . ?TN N N I MNNW T 8 aoo HO 00000000 To ? ooooo NrtltNrtplH O O O O 0_ v U Sx S -2 2H 9 f**- a 4 1 0 0 vi f l s s S S S S S sS s f& s S * H S S S S sS fsS S H S 's s i' S S f f * s S f p * aaa& o.ftA P.a sssss? ss**** (RMtlMUHtttt "if ? ? ? ? p ? ? 9 S 9 U*-*-*-! f r a | ? < s -5 Laaanaaa ** M>4 m M0<4 N*a4 M4 o0 o0 o0 o0 o0 0 0 h0 u* 00 0O 00 OO N<B4 M4 *4O4 144 N4O OO OO OO OO OO H HhX UUa Wu 4NHHhIt Af M4 HH U OO OO DO OO OOXOMOH OU Ot M E E i uuwuuui a 4 4 0 m 4 iOOBN mia U*400 O O (X (X o o o o o o O O O O O O O O O O O O 0e *O44 V0i Ut 0Hu 4*O 4O 04O X4O 44 0H 0*<04-444O<*44 OO4 OO4 OX4 OX0 OH4 UO4 OO4 O44 O144 O OOOOOO OOO 8444 O44 H44 A40 U40 4* 4A0 *O0 4H40U4* rtNIf Al NNIHM t 4WMH M4UHM 0 M H J O O * -4*0 g53535 MOlI* *I OHl UinI O OM HM u0 aU tm* 5? M*I* /" Mu 1U4t X t*** 1U4S OW MUtH* U teoto*o NH N14 M14MM MO H4 HO O> NO 1H4. OH HO U0*H4 OH * 0 *A*1 4 ir 1 M N X 4 0 ** M H H H <4 N M H < 4 H UNU HNH A 1NO41*O4 1Ua4UH14MUMtoMt uAM N O M4 W(4 *OO*AX IAAUM HM * t0-0H( 4 p U *N 0 1O4 UaH Au 4a iU N U0 *h 0u MO M* *0 04 0* 00 0* 1t*4 O4 * UW *M 4400**4 *0 *U*A(A4O0 a 3 3 ? ? 353553 555 55 55555 3 5 5. 35553 g|5 3 51 1 sO O 14 *O14 H*1 w4 *1-* H1 O .O 1 H1 >14 *4A*0O4 04**H4 M* Q u a n tify Compound S u m a ry K a p e rt to r 120, Ql-3 , r t l Sampl. U a t : e : \ M K M L Y M X \ n t e 2 . M O \ S M pl a O B \ O M 1 3 9 a taat nodlfled: Tue Jun 01 1*:1S:01 1*9 Method: C:\MA3SLTWX\rata2.PBO\M.thOO\OS01Mo Last modified: W e d Jun 02 OS: 4*: 03 199* Job Cede: Printed: Wed Jun 02 07:20:47 1999 Compound 4: IS Ha " t 060199020 2 060199021 3 060199022 4 060199023 S 060199024 6 060199025 7 060199026 9 060199027 9 060199028 10 060199029 11 060199030 12 060199031 13 060199032 14 060199033 15 060199034 15 060199035 17 060199036 19 060199037 19 060199038 20 060199039 21 060199040 22 060199041 23 060199042 24 060199043 25 060199044 . 26 060199045 27 060199046 28 060199047 29 060199048 30 060199049 31 060199050 32 060199051 33 060199052 34 060199053 35 060199054 35 060199Q5S 37 060199056 38 060199057 39 060199058 40 060199059 41 060199060 42 060199061 43 060199062 44 060199063 45 060199064 46 060199065 47 060199066 49 060199067 49 06Q199Q68 50 060199069 51 060199070 52 060199071 S3 060199072 54 060199073 55 060199074 56 060199075 57 060199076 56 060199077 59 060199078 60 060199079 61 060199080 62 060199081 63 060199082 64 060199083 65 060199084 66 Q60199085 67 060199086 68 060199087 69 060199088 70 060199099 71 060199090 72 060199091 73 060199092 74 060199093 75 060199094 76 060199095 77 060199096 71 060199097 79 060199498 60 060199099 61 060199100 82 060199101 63 060199102 64 060199103 65 060199104 86 060199105 Sappiali, t Text ethanol blank ethanol blank toxl20, rbl04199-eblk-2 COX120, rbl04199-lblk-2 toxl20, rbl04199-S ppb-2 toxl20, rbl04199*10 ppb-2 toxl20, rblQ4199-2S ppb-2 toxl20, rbl04199-50 ppb-2 toxl20, rbl04199-100 ppb-2 toxl20, rb!04199-2S0 ppb-2 t0X120, cbl04199-300 ppb-2 toxlZO, rbl04199-750 ppb-2 toxl20, rbl04199-1000 ppb-2 ethanol blank t0X120, lM-gl. 4/19/99 toxl20, 2M - 9 1 . 4/19/99 toxl20, 3H-gl, 4/19/99 . toxl20, 4M - 9 1 , 4/19/99 t o x H O , SM-gl, 4/19/99 toxl20, rbl44199-2S0 ppb-ce-1 ethanol blank toxl20, SM-gl, 4/19/99 toxl20, 7M-gl, 4/19/99 toxl20, (M-gl, 4/19/99 toxl20, 9M-gl, 4/19/99 tOX120, 10M-gl, 4/19/99 toxl20, rbl04199-2S0 ppb-cc-2, ethanol blank toxl2Q, llH-gl, 4/19/99 toxl20, 13M-gl, 4/19/99 toxl20, 14M-gl, 4/19/99 ' toxl20, 1SM-gl, 4/19/99 toxl20, rblQ4199-250 ppb-ce-3 ethanol blank toxl20, 6M-gl, a, 4/19/99 tOX120, SM-gl, Bad, 4/19/99 toxl20, 13M-gl, as. 4/19/99 toxl20, 13M-gl, Bad, 4/19/99 toxl20, rbl04199-290 ppb-cc-4 ethanol blank toxl20, 3K-gl, xa, 4/19/99 toxl20, 3M-gl, Bad, 4/19/99 toxl20, 41M-g3, 4/19/99, dlO COX120, 23M-g2, 4/19/99 COX120, 24M-g2, 4/19/99 toxl20, rbl04199-250 ppb-cc-S ethanol blank COX120, 25M-g2, 4/19/99 toxl20, 2SM-g2, 4/19/99 COX120, 27M-92, 4/19/99 COX120, 29M-g2. 4/19/99 toxl20, 30M-g2, 4/19/99 COX120, rbl04199-250 ppb-cc-S ethanol blank toxl20, 31M-g2, 4/19/99 tOxl20, 33M-g3, 4/19/99 toxl20. 34M-g3, 4/19/99 toxl20, 3SM-gl, 4/19/99 toxl20. 3SM-g3, 4/19/99 toxl20, rbl04l99-2S0 ppb-ee-1 ethanol blank toxl20, 37M-g3, 4/19/99 toxl20, 3SM-g3, 4/19/99 toxl20, 39M-g3, 4/19/99 toxl20, 40M-g3, 4/19/99 toxl20, 4 W -g3, 4/19/99 toxl20, rbl04199-230 ppb-cc-2 ethanol blank toxl20, 42M-g3, 4/19/99 toxl20, 43M-g3, 4/19/99 toxl20, 45H-g3, 4/19/99 toxl20, 46M-g3, 4/19/99 tox!20, 47K-g3, 4/19/99 toxl20, rbl04199-2S0 ppb-ce-3 ethanol blank toxl20, rbl04199-wblk-2 toxl20. rbl04199-lblk-2 tox!20, rb!04199-3 ppb-2 toxllO. xbl04199-10 ppb-2 t0x120, rbl04l99-2S ppb-2 COX120, rb!04199-50 ppb-2 toxlZO, rbl04199-100 ppb-2 toxl20, rb!04199-2S0 ppb-2 toxl2Q, rbl04199-S00 ppb-2 t0x120, rbl04199-730 ppb-2 toxl20, rbl04199-1000 ppb-2 S/2S/99 Amelia 0S249S: q u a n ti a te d and p r in t e d by h o i S/02/99 Page t Type Analyte Analyte Analyte Analyte Standard standard Standard Standard Standard Standard Standard 'Standard Standard Analyto Analyta Analyte Analyte Analyte Anelyte QC Anelyte Anelyte Anelyte Analyte Anelyte Analyta OC Analyta Analyte Analyta Analyte Analyte QC Anelyte Analyte Analyte Anelyte Analyte QC Analyta Analyta Analyte Anelyte Analyte Analyte QC Anelyte Anelyte Anelyte Anelyte Analyte Anelyte QC Analyta Analyte Anelyte Anelyte Analyta Analyta QC Analyta Analyte Analyte Anelyte Anelyte Analyte QC Analyte Anelyte Anelyte Analyte Analyte Anelyte QC Analyte Anelyte Anelyte Standard Standard Standard Standard Standard Standard Standard Standard Standard ltd Cone ** 1.00 1.00 1.00 1.00 1 e00 1.00 1.00 leOO 1.00 S.0S1 S. 0S1 5.024 S.031 S.01* 5.032 5.021 5.027 9.014 5.02S 5.003 . 1.00 5.024 5.01S S.04S 5.02 5.010 5.024 1.00 5.023 5.014 5.024 5.004 5.005 5.((21 1.00 5.02* 5.014 5.023 5.023 5.027 1.00 5.021 5.033 5.023 5.030 5.024 ' 5.01C 5.025 5.022 5.023 5.025 1.00 5.033 1.00 5. QIC 5.024 5.01S 4.55 5.013 5.015 1.00 5.042 5.004 5.019 5.012 5.019 5.010 1.00 5.025 5.021 5.042 5.019 5.005 5.014 1.00 5.022 5.049 5.01S S.02S 5.033 5.015 XeOQ 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.Q0 5.050 5.034 5.039 5.034 5.037 5.023 4.997 5.01S 5.01C 5.020 4.999 Ar* Cone, Flag* lDv 862 1055 1051 1057 1119 909 1047 906 907 899 972 0.92 bb 1.13 bb 1.12 bb 1.13 bb 1.20 bb 0.97 bb 1.12 bb 0.97 bb 0.97 bb 0.96 bb 1.04 bb 779 0.83 bb 73 0.93 bb 172 0.93 bb 909 0.97 bb 764 0.92 bb 870 0.93 bb 691 0.74 bb 730 0.78 bb 809 0.87 bb 700 0.75 bb 970 0.93 bb 953 1.02 b b 702 0.7S bb 684 0.73 bb 783 0.84 bb 667 0.71 bb 963 1.03 bb 768 0.82 bb 763 0.82 bb 696 0.74 bb 810 0.87 bb 948 1.01 bb 36 0.99 bb 77 0.94 bb 93 0.10 bb 466 O.SO bb 555 0.59 bb 886 0.95 bb 541 523 1219 779 536 9$ 0.58 bb 0.54 bb 1.30 MM 0.93 bb 0.57 bb 0.96 bb 591 985 509 . 457 546 814 . V. 517 483 630 466 471 940 0.63 bb 1.05 bb 0.54 bb 0.49 bb 0.59 bb 0.97 bb Q.SS bb 0.S2 bb 0.67 bb O.SO bb 0.50 bb 1.01 bb 659 0.71 bb 566 0.61 bb 535 0.57 bb 615 0.66 bb 534 0.57 bb 836 0.69 bb 913 >23 923 974 1061 108 978 843 7S8 764 850 0.99 bb 0.99 bb 0.99 bb 1.Q4 bb 1.14 bb 0.96 bb 1.05 bb Q.9Q bb 0.81 MM .0.82 bb 0.91 MM -8 13 12 13 20 -3 12 -3 -3 -4 4 -17 -7 -7 -3 -18 . -7 -24 -22 -13 -25 -7 2 -23 -27 -16 -29 3 -18 -18 -26 -13 1 -11 -6 -90 -30 -41 -5 -42 -44 30 -17 -43 -4 -37 5 46 -51 -42 -13 -45 -49 -33 -50 -SO 1 -29 -39. -43 -34 -43 -11 -2 -1 -1 4 14 -14 5 -10 -19 -18 -9 000721 b k \ Ch fat 4Ao> Quantify Calibration Raport to*120, fl1-3, rtl Calibration) Ci\MMOUfWC\rata2.R0\Curara\OOO199a U o t nodiflad: Wad Jan 02 07il(>0( 18 11 Prlntad: Wad Jun 02 07:20:91 1118 AaMlla 002490: q u a n tia ta d and p r ln t a d b y h o j 0/02/99 000722 Q uantify C alib ratio n Raport to*120, (1 -3 , r t i Calibrations C:\MJftanoc\rataZ.9IIO\Curvooa\090199a Laat aodlflod! (ad Jun 03 07:19:09 1*9 Prlntad: (ad Jun 03 07:30:31 19*9 9aja 3 alla 093499: piantlatad and p rln to d by ho) 9/03/99 000723 Q uantify C alib ratio n apace to*120, 1 -3 , r t l Calibration: C:\MM3UNX\rsta3.M\CtfrvaDa\0019fa Laat laodlflad: W a d Jun 03 07:10:0 1*9 rlntad: ad dun 03 07:30:31 If Pia* i Aamlia 0C2498: q u a n tla ta d and p rln ta d b y b o ) /0 3 /f f 000724 SOUP 020199: FACT Equipm ent L og 99014 Q uattro II, #6414E PAGE DATE: 06/08/99 ANALYST: drb STUDY NUMBER:TQX-120 M ATRIX:R at Liver DESCRIPTION: PQ AAanaIog_C_hcsk FACT M ethod: ETS-8-5.0 , Injection volume: 10 uL Cycle time: 9 min. E lectrode:.Z -SpPy------- M obile P hase: (A12.0 mM NH4CH3CQ2 (B ) M eQB-------- TN-A- o r stndrd num ber (A) 99012-10-9________ (B):TK-A:254fiL Prepared (date/by): (A1 06/04/99 drb ______ (B), Q6/03/29_dijb_ Expires: (At 10/99_______________ ( B ) _ lf lS L ----- Store at room tem p? @ or N Other:----------- :--------------- ---------- G u ard colum n: N one _______________ P art number: na_________ L ot number: na A nalytical colum n: Keystone B etasil ----------------------------------------- Size: 2 X SO mm_______________ _ Type: C18____________ Sphere size:J jjs a ---------- Part number: 0S5-701-2________ _ Lot number: P7LQ4 Serial num ber:Q481175Z A nalytical p aram eters: Drying gas fIVhrl: 350 ESI nebulizing gas (L /h r)J5 ____ Sheath gas (L/hr)_0 LC Flow rate: 300 uL/m in. B ack pressure: 55 b ar '' H PLC solvent g rad ien t: 9m in-2 lim s im iik L l io.oo 2 ) 1 0 0 .... 314.50 4 1 6.50 51 7.00 %B 40.0 40.0 .210 21Q_ 40.0_ 000725 M asslynx Sam ple List Sample List: C:\MASSLYNX\soup-rats.pro\SampleDB\060899a.SPL Printed: Tue Jun 0815:56:34 1999 Page 1 File Nam e 1 060899001 2 060899002 3 060899003 4. 060899004 5 060899005 6 060899006 7 060899007 8 060899008 9 060899009 F ile T ext M S F ile In le t File B ottle MeOH Blank Tox-120, RBL04199-UverBlk-1,4 /1 9 /! Tox-120, RBL04199-10 ppb - 1 ,4/19/ Tox-120, RBL04199-100 ppb -1 ,4 /1 9 , Tox-120, RBL04199-1000 ppb -1 ,4 /1 : MeOH Blank TO X -120,19M G 2 MeOH Blank T O X -120,35M G 3 POAA-51: POAA-51! POAA-51: POAA-51: POAA-51: POAA-51: POAA-51: POAA-51: POAA-51: 9m ln-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m in-2 9m In-2 9m in-2 91 1 2 3 4 91 5 92 6 4 V olum e S a m p le T C one A 10 Analyte 10 Analyte 10 Analyte 10 Standard 10 Standard 10 Analyte 10 Analyte 10 Analyte 10 Analyte 10 100 1000 000726 000727 a c u m i n a Katfced Sapore * Maehodi c>\nsiumx\poDV-iiua.M0vacaasa\aAk-si3-<ii' U i t Modifiadt t u A m 01 ll:55i54 U S * printad i Xu* A n 0* 15t00i44 I S M Solvent Stly ( alas ) j 0.00 Puaetioa : 1 M M of 1 M u i n i r < Uff- J Zatar Channel Delay ( Sacs ) i Spaa ( Daltona ) t Start Tina { Mina ) i Sad Time { Mina ) : Sapaata t Channal Paraat Daughter 0.03 0.00 0.00 9.00 1 Dwell (Seen) Coll Snargy (aV) Corn ( V ) 1 413.00 109.00 0.25 20 IS function s 2 m m of 1 Maas vaia ( Uff- ) Zntar Channal Dalay ( Saca ) < Span ( Daltons ) > Start Tina ( Mina ) i Sad Tiaa ( Mina ) s Sapaata i Channal Parant Daughter 0.03 0 .0 0 0.00 9.00 1 Duali (Saca) Coll Snargy (aV) Cona ( V ) 1 513.00 169.00 0 .2 S 20 15 function 3 M M of 1 M a i pair ( BSP- ) Zatar Channal Dalay ( Saca ) Spaa ( Daltoaa ) t Start ?Jj m ( M i n a ) i Snd Tiaa ( Mina ) i Sapaata * Channal Paraat Daughtar 0.03 0.00 0.00 9.00 1 Dwell SKI) Coll Snargy t.V) Cena t V ) 1 613.00 169.00 0.25 20 IS Puaetioa t 4 M M of 1 M u Pair ( SSP- ) Zntar Chaanal Dalay ( Saca ) s Spaa ( Daltoaa ) i Start Tiaa ( Mina ) i Snd Tiaa { Kina ) t Sapaata t Channal Parana Daughter 0.03 0.00 0.00 9.00 1 Dwell (Sac.) Cell Snargy (V) Cona ( V. ) 1 363.00 119.00 0.20 20 15 yuaotioa i 5 M M of 1 Naaa Pair C mar- ) Zatar Channal Dalay ( Saca ) t Span ( Daltoaa ) i Start. Tiaa ( Mina ) i Snd Tina { Mina ) i Sapaata * Channal Paraat Daughtar 0.03 0.00 0.00 9.00 1 Dwell (Sac.) Coll Snargy t.V) Cona t V > 1 463.00 169.00 0.20 20 15 Function f _ m o l of 1 Kuril Pair ( K4F- > Zntar Channal Dalay { Sk i ) i Spaa ( Daltoaa ) i Start Tiaa ( Mina ) Snd Tina ( Mina X t Sapaata * Channal Paraat Daughtar 0.03 0.00 0.00 9.00 1 Dwell (Sac.) Coll Snargy (V) Coaa < V ) 1 563.00 149.00 . 0.20 20 15 Function 1 7 uni of 1 H u . Pair ( U P - ) Zatar Channal Dalay ( Saca ) i Spaa ( Daltoaa ) i Start Tina ( Mina ) t Bad Tina ( Mina ) * Sapaata t Channal Paraat Daughtar 0.03 0.00 0.00 9.00 1 Dwell (Sac.) Coll Snargy t.V) Coaa < V ) 1 663.00 169.00 0.20 20 15 5 S o & fa Page 1 000728 Tuning Method Report Method: C :\MASSLYNX\SOUP-RATS. PRO\ACQUDB\PFOS Printed: Tue Jun 08 16:43:16 1999 o fo /o e /f Page 1 SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. Set Rdbk 3.00 60 5 0.2 150 250 3.01 -60 -7 153 252 Pressures Analyser Vacuimi Gas Cell Rdbk 2.2e-4 4.9e-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier \ MS2 Lto Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set Rdbk 14.0 14.0 2.0 0.0 52 650 Set Rdbk 15.0 15.0 45 2.0 0.0 40 0 650 43 38 43 000729 AM ELIA062498: FACT Equipm ent Log 99016 Q uattro n,# 6 4 4 8 PAGE DATE: 06/09/99 ANALYST: sah/mee STUDY NUMBER Tox-120, M ATRIX: ra t liver DESCRIPTION: IP FACT M ethod: cts-M -5.0________ Injection volume,lOuL Cycle tim e: 13.5 min. Electrode: Z-Spray M obile Phase: (A12.Q m M NH4CH3CQ2 (B1 MeOH TN-A- or stndrd num ber (A ) 99012-10-6_________ (B) TN-A-2647 Prepared (date/by): (A) 5/21/99 ias__________ (B1 6/7/99 sah Expires: (A) 11/99_______________ (B1 12/99________ Store at ropm tem pi [7] or N O ther G u ard colum n: None___________________ Part num ber na ' L ot number: na A nalytical colum n: keystone bctasil_____________ Size: 2 x 100mm "" Type: cl 8 Part num ber 105-705-2______ L ot num ber p7h!2 Sphere size: 5 um / Serial num ber 068640b A nalytical param eters: Drying gas (I/h r): 300 ESI nebulizing gas fL/hr) 15 LC Flow rate: 300 uL/m in. Back pressure: 80 b ar Sheath gas (L/br)_0 H PLC solvent g radient: p fb sl Tim e (m in.) IV 0.00________ %B 5___ ______________ 3 8.5_________ 51 11.0________ 61 12.0 . 71 13.5________ 1__ 90 90 5___ end 000730 M usU k M asslynx - Sam ple List S A K iA f c f _____: Sample U s t C:\M ASSLYNX\am elja-rats.PRO\Sam pleDB\060999a.SPL Printed: W ed Jun 09 15:01:191999 File Nam e F ile Text 1 060999001 methanol blank 2 060999002 methanol blank 3 060999003 tox120, rb!02229-H2Oblk-1 4 060999004 tox120, rbl02229-Llverblk-1 5 060999005 tox120, rbl02229-5ppb-1 6 060999006 tox120, rbl02229-10ppb-1 7 060999007 tox120, rbl02229-25ppb-1 8 060999008 tox120, rbl02229-50ppb-1 9 060999009 tox120, rbl02229-100ppb-1 10 060999010 tox120, rbl02229-250ppb-1 11 060999011 tox120, rbl02229-500ppb-1 12 060999012 tox120, rbl02229-750ppb-1 13 060999013 tox120, rb)02229-1000ppb-1 14 060999014 methanol blank 15 060999015 tox120,106F-G 1-250ppb-m s, 2/22/99 16 060999016 to x 1 2 0 ,106F-G1-250ppb-msd, 2/22/99 17 060999017 tox120,3M -G 1-250ppb-m s, 4/19/99 18 060999018 tox120,3M -G1-250ppb-m sd, 4/19/99 19 060999019 tox120, rbl02229-250ppb-cc1 20 060999020 methanol blank 21 060999021 to x120,153F -G 4,2/22/99 22 060999022 to x120,154F -G 4,2/22/99 23 060999023 to x120,155F -G 4,2/22/99 24 060999024 tox120, rbl02229-250ppb-cc2 25 060999025 methanol blank 26 060999026 to x120,157F -G 4,2/22/99 27 060999027 to x120,158F -G 4,2/22/99 28 060999028 to x120,159F -G 4,2 0 2 /9 9 29 060999029 tox120, rbl02229-250ppb-cc3 30 060999030 methanol blank 31 060999031 to x120,57M -G 4,4/19/99 32 060999032 to x120,58M -G 4,4/19/99 33 060999033 tox120, 59M -G 4,4/19/99 34 060999034 tox120, rbl02229-250ppb-cc4 35 060999035 methanol blank 36 060999036 to x120,61M -G 4,4/19/99 37 060999037 to x120,62M -G 4,4/19/99 38 060999038 to x120,63M -G 4.4/19/99 39 060999039 tox120, rbl02229-250ppb-cc5 40 060999040 methanol blank 41 060999041 to x120,169F -G 5,2/22/99 42 060999042 to x120,170F -G 5.2 0 2 /9 9 43 060999043 to x120,171F -G 5,2 0 2 /9 9 44 060999044 tox120, rbl02229-250ppb-cc6 45 060999045 methanol blank 46 060999046 to x120,173F -G 5,2 0 2 /9 9 47 060999047 to x120,174F -G 5,2 0 2 /9 9 48 060999048 to x120,175F -G 5,2 0 2 /9 9 49 060999049 tox120, rbl02229-250ppb-cc7 50 060999050 methanol blank 51 060999051 tox120,73M -G 5, d 2 5 0 ,4/19/99 52 060999052 tox120,74M -G 5, d 2 5 0 ,4/19/99 53 060999053 tox120,75M -G 5, d 2 5 0 ,4/19/99 54 060999054 tox120, rt>l02229-250ppb-cc8 55 060999055 methanol blank 56 060999056 tox120, rb!02229-H2Oblk-2 57 060999057 tox120, rbl02229-Liverblk-2 58 060999058 tox120, rbl02229-5ppb*2 59 060999059 tox120, rbl02229-10ppb-2 60 060999060 tox120, rbl02229-25ppb-2 Pagel MS File PFHS PFHS PFHS PFHS PFHS PFHS PFHS PFHS PFHS PFHS PFHS PFHS PFHS PFHS PFHS PFHS PFHS PFHS PFHS -PFHS PFHS PFHS PFHS -PFHS PFHS PFHS -PFHS PFHS PFHS PFHS PFHS -PFHS -PFHS PFHS PFHS -PFHS -PFHS -PFHS -PFHS -PFHS -P F H S -P F H S -PFHS -PFHS -P F H S -P F H S -P F H S -P F H S -P F H S -P F H S -P F H S -P F H S -P F H S -P F H S -P F H S -P F H S -P F H S -P F H S -P F H S -P F H S In le t F ile . pfbsl p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l pfbsl p fb s l p fb s l pfbsl p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l pfbsl p fb s l p fb s l p fb s l p fb s l pfbsl pfbsl p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l p fb s l - 000731 B o ttle 91 91 1 2 3 4 5 6 7 8 9 10 11 92 12 13 14 15 81 92 16 17 18 82 93 19 20 21 83 93 22 23 24 84 94 25 26 27 85 94 28 29 30 86 95 31 32 33 87 95 34 35 36 88 96 37 38 39 40 41 A iiiih k U M Massiynx - Sample List X M U / n f t l - ___________ : Sample List C:\MASSLYNX\amelia-rats.PRO\SampleDB\060999a.SPL Printed: Wed Jun0915:01:191999 File Name 61 060999061 62 060999062 63 060999063 64 060999064 65 060999065 66 060999066 File Text 10X120, rb)02229-50ppb-2 tox120, rbl02229-100ppb-2 tox120, rb!02229-250ppb-2 tox120, rW02229-500ppb-2 tox120, rblQ2229-750ppb-2 tox120, rb!02229-1OOOppb-2 v/v/vy /y ? ? a Page 2 MS File PFHS PFHS PFHS PFHS PFHS PFHS Inlet File pfbsl pfbal pfbsl pfbsl pfbsl pfbsl Bottle 42 43 44 45 46 47 000732 A n tiO i M S A r i fr/a/91______ Tuning Method Report Method: C :\MASSLYNX\AMELIA-RATS.PRO\ACQUDB\PFOS Printed: Wed Jun 09 1 5 :0 1 :3 5 1999 0/1/9? ' /n & ? - Page 1 SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. Set Rdbk 3.00 15 5 0.2 150 250 2.98 -60 -5 150 251 Pressures Analyser Vacuum Gas Cell Rdbk 1.4e-4 4.9e-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 56 650 Set Rdbk 15.0 15.0 30 2.0 0.0 40 0 650 47 37 44 000733 Amtitk M W SM U Scanning Method Report Methods C.-lMMSLXKXVMSKUh-RhTS .PRO\*CQUDS\ taat Modified: Wad Jun Of 14:17:1? I M S Printed: ad Jon 0 19:01:0 199 /a M -ms Solvent Delay ( mlna ) i 0.00 function I 1 M8M of 2 Mass t a i n ( ISP- ) Inter Channel Delay { Sees ) t Span.( Daltons ) > Start Ties ( Nina ) i End Tina ( Xina ) : Repasts t Channel Parent Daughter 0.03 0.00 0.00 13.90 1 Dwall (Secs) Coll tnsrgy (aV) Co m <V ) 1 299.00 0.00 0.00 2' 299.00 99.00 0.40 49 45 <0 60 funotion s 2 M M o f 2 Maas Pairs ( ISP- ) Inter Channel Delay ( Secs ) t Span ( Daltons ) > start Ties ( Mins ) i End Tina ( Mins I : Repeats i Channel Parent Daughter 0.03 0.00 0.00 UeSQ 1 fiNill (Sacs) Coll Energy lev) Co m * (V ) 1 399.00 10.00 0.40 2 399.00 99.00 0.40 43 45 60 60 Saga 1 # 000734 r fiv. i ; u r t i A K ^ v i L W SUMMARY FORM Date: M ila 0(34*8: quantitad and p rin ta d b y bo} < /1 0 /M 01 (*J U M l) WA A*Al *f l* UA**U*t *4 H OUVUl< d1 UW NWHW0 UV M0 -M4M0MU IH4 M A U * U N #-* O 10 O I A 40A oooo oA<4 ooo se o e e oe eooc o o o o e o4 c 004 10 to I IOI4WU410to V 4UUUUMMNMMe o0e4 , 10(0 O 10 oo oto tow oov OO O Oc AOVKI sa* 1 X 4 HOOOa Oo AA OO to IA to 10 to 10 10Atlft O .O IO O 10 O Oo Oo to OI 01 .ACO* eoooooooo oo< o o o o o o o ______Ae__o_A_e__ 10(010101010101010101010 10101010101010'' "> 1-0 1-0 1 1* VtftfVMAIOV OOOOOOO e-- e>ioo oio rid Ul (0 A A A A * M O IO <I I*U N H 0 oooo AA O10 1O0 10 o O o O 10 O 10 10 1o0 1o0 uu e o U io oc Ul i0 m W A i 3 0 0 0 0 0 0 0 0 0 OOOOOO o" to to> WAe0MloA0IoOoAAw0OIwoA0lOvoAOM0i MOpoA0ItMoA0OatIoA0fwPA0o1O0 A O 10 to to MO A O to to to OM A O to to to ON AA OO 10 to 10 to to to ON ON A O 10 10 to OH lUNHOVBslAU) 0UNHOW O A O to to to HO O OOOOOO AAAAAA OOOOOO to to to to to to to to to to to to to to to to to to OH OH Oh Om Oh Oh *JO O0UM OO Ao oA 1010 to to 10 to OO OOOOOO AAAAAA OOOOOO to 10 10 to 10 to to to to to to to to to o io to io OOOOOO OOOO OO oO oO oO to O JA U A U M M sssssssssssr t r t r t r t r t r t r t r r n r r r f MeoNMooMoMoNMoNoMoMoMe aTNoHMMoMMeoMN ooooooooooo HTO UJTOT0 UTM THO OT jTaTMbTUs TMK THR . 1 1 MtTK . . . . J MMM H ( MMMN ft M ff KKKXftXrbKr Xon rXot WfitbrXf orMr brMt ofMt MiftotMt foKt Mo<*oXr t OMNMMN g oopogo ftrtv tftftB ftftftftftrrre rtftftft t|f9B i8faM08Ma0M8M*0MM80MMS0MM9OtiMSOra M8HOa M8HaOM8MaOMSMOMM8OM8MOM8NOHaM8OMa8MOMa8MOH l i t s & S t s s S Uu2 *UwiUMrM.fNf1 uM0u0MuMeJ rM(MHr Wt*MHHH1HHNHH' IB H * i % a rs r !CSC f c cc CO ta a U a 0S2499 : q u a a tla ta d and p rln ta d by i a j 9/1 0 /3 ffT T Y T T T T T T IP MI M1 M1 N1 M M M KM MI ,&ea ?ssg Ari sIHW0WsHVIUH\0> MMM M S S . S ga I " " " f t S t 4ttv mhOOmm Omh Omh Omh Omn Omm OmmQmhOmhOmhfthh5ftH K K K K K m KKKKK"'^ 5A Ai f Y f Y Y Y Y f Y Y f E * E.Sl Ht 1*M Ut} 58S I . .I rc s ! S SS t l~ r ?ir }ifai" 3 S Il 0X0] Sa S s is ! M ft Oft :: vv pi mjp o 9 O tilllllli--- 5553 33333hIiII3333H I H f ! H i i 8 E i 8 r ' H s r r , H S { * H E r , E i U i { H H i r i i f 3333 3333 3333 3333 3333 3333 HsytMH SSSSSSS SSSSS8888 I ' ' > W S8 M 8 ggg MM 8 .8 W .8 gggg < t t v w w w w www o |S3g i i g s ssss ssss is s g -s WM 88 g HftdINH .8 8 8 8 8 8 8 8 . ggggggggg # < w w w w w w w w w w s gsssg sssssgsgsl o I 3 iS S S S s b " H i " S = s s s : ; 3 SSSs st . s s H ^ S s s s a s S O O I s S s S s s S S S i ' s B S s H i t s s s 5 5 = s ' : l l ' i I SSs s s O sssssss Sags sss s s ts 58So sas? s bssss ssssbcbsss >3 ggggggg . gggg gggs ggg gggg gggg g g ggggg gggggggjfg I CO WI HHt HfIt fIt O O f t MoI . rfj- MHI HO I UI H MM l m w I WUtMf HuOHwM ? f e } > L > fe j- _________________________ ______________________ _ ______________________________ a u itie ir CaU bcm tlon lU p o rt t U O , and f O i fan 1 C a l l t e a t i o n i O V a M M n o ftaaar t l a B d . n a v e t nOOVOOOOW* l u t a o d lfla d i I t a Jttn 10 0 7 iU il7 1999 T rlatadt I t a Ota 10 0 7 itt< 3 S 1199 t a l i 0<34M> q u a n tla ta d and f r l a t a d b y b a l 9 /1 0 /9 9 000738