Document v1oMdLBnb1L3X5L0vgVxM8d2Y

gGH& - 0 2 0 0 - $ 1 5 J R zz6 -0 % lys -y Laboratory Report, Analysis of FCs in Samples of Children's Sera, May 21, 1999 The data submitted on perfluorooctanesulfonate contains analytic data when certain general conditions have been met. These are that final analytic data is available and that if this data is a component of a study, a report exists that combines the data and other parts of the study. Data that has not been integrated into a report, or pilot data, has generally not been included in the submission. The attached is pilot data showing results from a limited number of human blood samples (pediatric samples from the University of Minnesota). This pilot was meant to determine that the analytic technique could be used on a small volume of serum. Although fluorochemical concentrations were above detection limits, no conclusions can be drawn from such a limited number of samples. The planned study will contain results from over 600 pediatric samples. The samples in this study will be run in a contract lab using a different blank under GLP conditions. The plan for this study has been previously submitted under cover of the April 21st letter to EPA. Cj r3i O 1 -o rn -C O --ir n o rn ;r- ; o PO cr y> E P A - O T S 000811798Y Q o a iiT ia Y ci, o >w Cl' <i~> Aj ^r A.- C l! A 1 j 1 7i C042S9 3M Environmental Technology and Services PO Box 33331 St. Paul, MN 55133-3331 612 778 6442 Laboratoiy Report A nalysis o f FC s in Sam ples o f C hild ren 's Sera L aboratory R eport No. FACT-GEN-011 W 1724 Testing Laboratory 3M Environmental Technology & Safety Services 3M Environmental Laboratoiy Fluorine Analytical Chemistry Team (FACT) 2-3E-09 935 Bush Avenue, St. Paul, M N 55106 Laboratory Contact Kris Hansen, Ph.D. Bldg. 2-3E-09 P.O. Box 3331 St. Paul, M N 55133-3331 Phone: (651)778-6018 FAX: (651) 778-6176 Requester Geary Olsen and Jean Burris 3M Company Occupational Medicine 220-3W-05 St. Paul, MN REPORTDATTE: 05/21/99 004290 BEST COPY AVAILABLE JM ENVIRONMENTAL LABOR/ITORY REPORT NO. FACT-GEN-0U Introduction Samples were analyzed to provide a quantitative determination of PFOS and PFHS in a small number of samples o f sera collected from children between the ages of 6 and 12. Additionally, samples were screened to provide qualitative data on the presence of several other fluorochemicals including PFDS, PFOSA, PFOSAA, M 556, M570, POAA, M463, and M513 (Appendix C contains a list of acronyms). Less than 100 pL o f sera were available for analysis. This small sample volume posed analytical restrictions and method detection limits for this study are significantly higher than reported in earlier studies. Sera samples were extracted using an ion-pairing extraction procedure. The extracts were quantitatively analyzed for PFOS and PFHS using high-pressure liquid chromatography/electrospray tandem mass spectrometry (HLPC/ESMSMS), and evaluated versus an extracted curve. Qualitative analysis was conducted by comparing peak response in the samples to that obtained from standards,'when possible. If standard m aterial was not available, compound identification was based on reasonable HPLC-retention time -- and predicted mass spectrometer response. Analytical detaftraifravailabre in the study binder maintained by FACT. Despite the increased detection limits that resulted from the small sample size, several fluorochemicals were detected in these sera samples. PFOS, PFHS, PFDS, POAA, and M463 were detected in each of the samples . analyzed; for these analytes, the estimated detection limit is 3 ppb. PFOSAA, M556, and M570 were detected in some o f the samples and the detection limit is estimated to be approximately 5 ppb. PFOSA and M 513 were not detected in any sample above the estimated detection limit of 8 ppb and 12 ppb, respectively. The average PFOS concentration was 54 ppb, covering a range of 31-115 ppb. These values are slightly higher than the average values observed previously for adults and some part of that (up to 10%) may be due to improvements to the modified method used to extract these samples. The average PFHS level determined in these samples was 35 ppb across a range o f 5-100 ppb. This average is approximately 10 times higher than the levels previously observed in a small set of adult sera samples. In those samples, die highest value determined in a non-3M worker was 13 ppb. It is unlikely that the minor' modifications made to the analytical method could account for this dramatic difference between the two groups o f samples. Although rigorous quality control measures and 3M Environmental Laboratory Standard Operating -- Procedures were followed, the acquisition o f this data was not necessarily collected according to applicable Good Laboratory Practices. This data is not suitable for distribution to arty government agency in defense o f product suitability or safety. D ata presented here is the highest quality data available at this time. 2 Sam ple Receipt On 4/27/99, Jean Burris o f 3M Occupational Medicine delivered seta samples to the Environmental Lab. Environmental Lab personnel initiated a chain-of-custody upon receipt of the samples. 2 H olding Times There is no holding time criteria associated with these samples for LC/ESMSMS analysis. REPORTDATE: 05/21/99 004291 best m mum JM ENVIRONMENTAL IABORATOR REPORTNO. FACT-GEN-011 m M ethods - Analytical and Preparatory A nalytical m ethods ETS-8-4.0, Extraction of Potassium Perfluorooctancsulfonate or Other Fluorochemical Compounds from Serum or Other Fluid for Analysis Using HPLC-Electrospray/Mass Spectrometry MODIFIED to accommodate small sample size. Reagent volumes were reduced and aqueous extracts were triple rinsed with MtBE. These modifications may result in slightly better analyte recoveries than those achieved using the original method ETS-8-5.0, Analysis of Potassium Perfluorooctanesulfonate or Other Fluorochemical on Serum or Other Fluid Using HPLC-Electrospray/Mass Spectrometry MODIF IED for PFHS determination by comparing PFHS samples response to PFOS curves, as no standard PFHS was available. This substitution is likely to result in a slight UNDER estimation of PFHS levels. Sam ple preparation - aqueous sam ples, HPLC/ESM SM S: ion-pairing extraction -- ' - Analyte is extracted from asam pfe matrix with iorrpairiri^reapnt [Jetfabutyl ammonium hydrogen sulfate (TBA)] in a pH-controlled environment The cationic reagent selectively targets anionic fluorochemicals. Once the anion-TBA pair is form ed the analyte is transferred into a non-polar organic solvent (methyl-ferfbutyl ether), dried, and reconstituted in methanol for MS analysis. HPLC/ESM SM S: for detailed qualitative w ork In HPLC, an aliquot of extract is injected and passed through a reverse phase liquid chromatographic colum a 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 8.0 minutes. Retention times between a standard PFOS solution and the analyte extracted from sera 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 of molecular ions, is generally operated at relatively mild temperatures. Molecules are ionized, and a primary ion, characteristic of the analyte, is selected. This ion is bombarded with high-energy gas; subsequent collisions create smaller secondary ionic fragments unique to the primary ion, which are detected. For example, for PFOS (CjFpSQO analysis, ion 499 is selected as the characteristic primary ion. This ion is fragmented into other ions such as 80 amu (corresponding to SQO> and 230 arau (CjFfiS^"). Each of these secondary fragments is detected and can be used to differentiate PFOS from other compounds that m ight have the same characteristic 499 amu primary ion, but different chemical compositions and secondary ion fragmentation patterns. 5 Analysis 5.1 C alibration For quantitative determinations, a mid-level, extracted matrix calibration check standard is analyzed every 5 samples to monitor instrumental drift. Calibration check standards are compliant if instrumental response is within +/-10% o f the expected value. Quantitation of the target analytes is based on linear regression analysis (weighted 1/x) of two extracted matrix curves bracketing each group of samples. Quantitation of each analyte is based on the response of one or more specific daughter ions using the multiple response-monitoring mode of the instrum ent REPORTDATE: 05/21A/J C04232 BESTcopy AMUABIE JM ENVIRONMENTAL IABOMTORY REPORT NO. FACT-GEN-0U 5.2 Blanks Two extraction blanks, utilizing water as surrogate matrix, are extracted with each batch o f samples. Additionally, two samples of blank matrix or surrogate 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-hydro perfluorooctane sulfonate is used as a surrogate in this analysis. Surrogate response is monitored to confirm gross instrumental failure. 5.4 M atrix Spikes Duplicate matrix spike analyses utilizing all target analytes for which quantitativejla ta is presented were prepared and analyzed for one control anim al For sera analysis, recoveries were within die acceptable range o f 85-115%. 5.5 L aboratory C ontrol Samples Laboratory Control Samples are not a component o f this study. 5.6 Sam ple R elated Comments Due to limited sample volume, it was not possible to conduct matrix spike studies on any o f these samples. Although the current understanding of the analytical methods indicate that rabbit serum is a suitable surrogate matrix, matrix spike studies for this matrix are recommended. Standard materials for PFDS and M463 were not available for compound identification at the time of analysis. Compound identification is based on reasonable retention time and mass spectral data consistent with compound structure. $ Data Summary Despite the increased detection limits that resulted from the small sample size, several fluorochemicals ware detected in these sera samples. PFOS, PFHS, PFDS, POAA, and M463 were detected in each o f the samples analyzed; for these analytes, the estimated detection limit is 3 ppb. PFOSAA, M556, and M570 were detected in some o f the samples and the detection limit is estimated to be approximately 5 ppb. PFOSA and M 513 were not detected in any sample above the estimated detection limit of 8 ppb and 12 ppb, respectively. The average PFOS concentration was 54 ppb, covering a range of 31-115 ppb. These values are slightly higher than the average values observed previously for adults and may be due to improvements to the modified method used to extract these samples. The average PFHS level determined in these samples was 35 ppb across a range o f 5-100 ppb. This average is approximately 10 times higher than the levels previously observed in a small set o f adult sera samples. In these samples from adults, the highest value determined in a non-3M worker was 13 ppb. It is unlikely that the minor modifications made to the analytical method could account for this dramatic difference between the two groups of samples. This report reflects the most accurate data available at this time. 7 D ata/Sam ple Retention Samples and extracts will be retained for future evaluation if necessary. REPORTDATE: 05/21/99 004293 3M ENVIRONMENTAL LABORATORY REPORT NO. FACT-OEN-OU 8 Attachments 8.1 A ttach m en t A : Q uantitative Results o f PFOS and PFHS Determ ination 8.2 A ttach m en t B: Q ualitative Summary o f FCs identified in Samples o f C hildren's Sera 8.3 A ttach m en t C : Table o f FACT Acronyms 8.4 A ttach m en t D: Chain o f Custody 8.5 A ttach m en t E : Analytical D ata for PFOS and PFHS determ ination s% / * < * A * * * X-v-v X y tt f s t X* . m A A V / . V f * * v* ** V* \ ' - ' t --5 ' ' 7 - ; - * ',^ ' ''V ' S ig n a tu re s *" >> ' i' > ^ W .V W iW .W A W m V .m V M V .W .V A V .W V A V A '.W A V M m W ^ W M W .V .V .V M V .W M W .V A '/ M W W W iW W W i'i'K S V .V .W W A W / M ^ V W < V .V W * V A V / M W K ,. W A ^ A W ^ ^ ; > f f ? W M r K ,WK /4 CL V O s Lisa Clemen, Analytical Chemist / X L / X - -------------Kris Hansen, Ph.D., Study Director s /a ilw D ate /Z J /S ? D ate REPORTDATE: 05/21/99 004294 G?"' " l l Serum Data Study Product NumBcifTest SuBstancc> Matrix Method/Rcvaion: Analytical Equipment System Number Instrument Software/Venion: Filename: R-Squared Value: Slope Y-Intexcept Date o f Extraction/Analyst: Date o f Anatyiia/Analyit: Date o f Date Reduction/Analyst: S am p le D ata OEN011 PFOS and PFHS Extraction front serum N/A H Saun ETS-8-4. end BTS^-5 0 Amelie 062491 Masslynx 3.2 Saa Intmg to tha right See Attachment! Sea AttachnuaiU Sea Attachments 04/24/99 RWW 04/30/99 HOJ 05/03/99 HOI Filanamea 4. Sam ples Sample* MS/MSD PFOS 04309901S-30 NA 043099031-33 PHFS 043099016-30 NA 043099032-33 D ila ti 1/1.1/1.1/1.1/1 1/1.1/1.1/1,1/1 in. m. l/i, i/i Seram Group Dace S a u p li # Extraction VaL Ratto PFOS D ilu ita Method Blk Matnx Blk QC-2S0 ppb H 20B lk-l H 20 Blk-2 RBS04289-SBIk-t RBS04289-SBIk-2 RBS04289-MS-1 Pactar 1.0 1 1.0 1 1.0 1 1.0 1 1.0 1 GENOU RBS04289-MSD-2 9394 9395 9596 9397 1.0 0.5 0.4 0.4 0.4 1 1 1 1 1 939S 0.4 1 9399 9400 9401 9402 0.4 I 0.4 1 0.4 1 0.4 1 9403 0.4 1 Limit or QuatMation (LOQ) PFOS - 4.93 ng/mL, PFHS - 4.93 ng/ntL Method Detection Linus (MDL) PFOS 2.4 ng/rnL. PFHS " 2.4 npfatL PFOS Cooc. ag/eeL 0.00 0.00 0.00 0.00 281 256 14.1 19.5 25.5 13.1 12.3 10.7 21.0 15.2 46.3 26.0 PFOS Reported e/m L <MDL <MDL <MDL <MDL 113% 103H 0.0312 0.0557 0.0638 0.0327 0.0352 0.0305 0.0601 0.0380 0.116 0.0744 Average PFOS l/n L <MDL <MDI. 108% USD Std. Dev, <MDL <MDL 0.0711 PFHS D ilutU a Factor 1 !. 1' 1 1 1 1 1 1 11 O.OS37 -- LL.S0.0 0.0269 1 PFOS - PcriiuonooclanecrlfonaU PFHS * FetOixnohexenesulIbnete PFHS Cene. c/utL 0.00 000 000 0.00 NS NS 6.48 16.7 19.9 5.23 I.II 2.39 37.6 14.9 9.17 16.4 PFHS Reported be/kiL 000 000 000 000 NS NS 00144 0 0479 00498 00131 00052 0.0068 0.107 00372 00229 0.0469 Date Entered/By. Dele Verified/By: 05/03/99 LAC OS/21/99 kjh i Average PH IS ut/mL 000 000 NS 0 0352 RSD Std. Dev. 000 000 NS 87 4 0 0307 I oo 10 CjD BEST copy AVAILABLE ETS-tt-4 rt 3M Environmental Lab - Fluorine Analytical Chenistry Team APPENDIX B Q ualitative Sum m ary of FCs identified in C h ild ren 's S era Sam ples Sam ple # PFOS (ppb) P F H S (ppb) 9394 9395 9396 9397 9398 9399 31 56 64 33 35 31 14 48 50 13 5 7 9400 9401 60 38 107 37 9402 9403 116 74 23 47 X - detected PFDS X X X X X X X X X X POAA M463 XX XX XX XX XX XX XX XX XX XX ** = not detected PFOSAA X X X ** ** ** X ** X X M 556 ** ** X X X X ** ** X X M$70 X X ** ** ** X X ** X X estim ated detection lim it for PFDS, POAA, M463 is 3 ppb estim ated detection lim it for PFOSA is 8 ppb estim ated detection lim it for PFOSAA, M556, M 570 is 5 ppb estim ated detection lim it for M513 is 12 ppb i ? i BEST COPYAVAILABLE CO C5 3M Environmental Lab - Fluorine Analytical Chemistry Team P F S 's PFHS C 6FI3S 03PFOS C 8F17S03PFOSA C8F17S02NH2 PFOSAA C 8 F 17 S 0 2 N ((C H 2 C H 3 )(C H 2 C 0 0 ))M556 C 8F17S02N ((H )(C H 2C 00))M570 C 8F 17 S 0 2 N ((C H 3 )(C H 2 C 0 0 ))- j PFDS C10F21SO 3- ** P F C A 's POAA C7F15COOM513 C9F19COOM463 C8F17COO- ** PFS = perfluorinated sulfoante PFCA = perfluorinated carboxylic acid ** no standard material available for confirmation; 004297 Lisa A. Clemen ^ 04/27/99 04:55 PM Environmental Technology & Safety Services (6 5 1 )7 7 8 -5 5 6 8 3M Building 02-3E-09 PO Box 3331 S t Paul, MN 55133-3331 Fax: (651)778-6176 BEST COPIf AVAILABLE To: Kris J. Hansen/US-Corporate/3M/US Kari J. Rambo/US-Corporate/3M/US Grant A. Paui/US-Corporate/3M/US cc: Subject: GEN011 Sample Receipt On 04/27/99 we received 10 special H. samples from Jean Burris of Occ. Medteal.- These samples have been given project # FACT-GEN011, Lab request number W1724. Samples were received cold and have . ,, been stared in Freezer 9 at -20 +U 10C-. ------------- Lisa 004233 Environmental Laboratory Request Form Lab Request No. t ` ;V It Date Received Page ; of / Address 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 Nam V * P,)m i Projdct Description (40 Characters Max.) Location R e q u es ter Phone No. fio & M . 73/ V L I L man Q ,. Is this a TSCA B(d) project? (See beck side fo r Instructions) Dept. No. (Main) Sub. Acct. MUST BE CHECKED Q Yes Purpose of Testing No W l Oate<Needed f O Routine Plant Code C iass/Job/Pibjact No. O I0 5 3 5 D O Environm ental Lab Project Lead Expected Comp.ct.cn Dale Planning Status Quality Review C lass/Priority Date Snipped RCRA ' TSCA CWA CAA SDWA MSDS Salary Concems/Special Handling Comments JC . t t iiii.r. o t C I ' M i J - j ^ S'iljiU. nu/b(>'J , .(1_ Tests Required Sample No. (Range 0-999) Sample Code (12 Character M ax)' Sample Date & Time (M M /DD/YY, HH:MM) Sample Description (12 Character M ax)* 3M I.D . (11 Character Stock No.) om puterC ode GtT Avail. Date IDue Date K ' j H 0 |)(:t OP O Cr IT CO CO Form 10620 - P - PWO White Environmental Lab Archives Pink - Contractor Canary - Disbursements Copies To: ,j-j | \(^ 409 Chain of Custody Record 3M Environmental Laboratory 11437 Form 3 5176-PWO 3M Facility 3M Project Title Address t ! A -0 l 3M Facility Contact )y > / f v / / v City. State. Ztp Code 3M Telephone Number --- :___________ 'Ll_____!_______ . } 1 Sampled By (Print) Sampler Signature Item # 1 2 3 4 5. 6 7 8 9 10 11 12 13 , |i :> 1 Sample Description *- ' . ...... ... - Contractor Dale /7/ Date Time Matrix </ .--_;_Li_ I Number Containers of each Preservatives 8n oZZ 04 X \/ __ None NaOH Total Containers of Each Hem 3M Requester ),: . ; 3M Project Lead 1. ' . ' 3M Project Number i 3M Department NumDer /f Lab Requesttfempiate Number * ^ Sam p les Split S e e A ttachm ent Comments // ,H' / '* 1 ' ' / DO n ^9 f . w 25 ! a t VH-'- ' i= 1 L _____________________________ f e mm r i Item # r^ 1 l| CO Relinquished By/Affiliation / 1 */ Time 1 Date Shipped Via ,ijt- Received By/Affiliation ,1 1 * Time Date BEST COPYAVAILABLE Extraction Worksheet ETS-8-4.0 1 i<3 ni i J Study tt / - z a / o / ) Box H M atrix Surrogate Std approx. ppm actual /o o ppm FC-Mix approx. 0.5 ppm actual ppm t f r t i t - ' J j 7 -/.- / l k -N }- ____ s s / _______ ' 'lU-H i - /a J FC-Mix approx. 5 ppm actual ppm - FC -M ix approx. 50 ppm actual ppm ft P t c / J - Z r A - Date and Initials for Std. or C om m ents 1 .... ~ /C n .i * J'7n. l - h i- 1 .r J )o J. / . 1_______ 1 - 7\,.U-h L- 1 -/ cjt.i-i'll- -2fA fA -tl -2?-ec2. J1 - /is Jf ? ./? )- 0 9 * ! $ IIS ' - , ?~- / 9 j '? - A ,0X + . / < o , iJ S ,7U <7l9< p , D 7 U . 9J??Zj / j - , ]T ~ lr /. V J . ____ ik/ - - - - - __ ,,> - - - - - - - - - - - - - i / r j ) -------------- w5 al/ - -y - 1 Study num ber w hsrs th original worksheet is located. Blank /L U ,) std* fi. . ........ . ..................... amount = JZH. mL Serum Extraction Method j / t i s - s - <ZZ l Date & Initials Vortex IS sec. Pipette Matrix Volume U T ml Pipette 1 ml o f 0.5 M TBA, pH -W / Pipette 2 ml o f 0.25 Na?COV0.25M NaHCOt buffer Std. # / / ~ / J ? Dispense 5 ml of rpethyl-t-butyl ether (jQ TN-A- 3 9 S~ 9 Shake 20 min. S /> s s J ^>C Centrifuge 20-25 min. Remove a 4 iuL allUUOt ofrgTThrtayer C/) Centrifuge speed: S S ~ Q 2 Y /J i'iS tfe - A t t u i Put on Nitrogen Evaporator to drvness Evaporator #: Temperature: /*'* >* y / * / * *w Add methanol Vortex 30 sec. Volume Z 2 ml TN-A- Filter using a 3cc B-D syringe with a 0.2um filter into a 1.5 ml autosamole vial f 1 2 __________ M S/M SD / X Cont. Checks: Spiked S uL o f a Sc ppm std ( 9 ^ / 2 -A i- ) for a final concentration o f O , t ` ppm. M S/M SD used sample J ' *-/1 3 S > t Cont. Checks used same matrix as for std curve. Surrogate Standard: Spiked uL o f a _____ ppm std (___ __) to all sam ples, standards, and blanks ^ A/ / / s ' ^ / / --J j i / ' j h tfs C / f JJ Attachment A r> s / f J > 2 - J i . ~ y / / i r yy /. `- ? j ) /J u (/j * ' , /w/f ^-5 ><* f 7/*^, / .o. YJ* '/ > . > /- > / r s Z - A - J j ' ? / *I ._ T. / " > , o/A l i - r # ^=- j i*. e & j j - A /<><'' j j/ i < - 5* '< ' * * 9 ' ' ETS-8-4.0 7 Page 10 o f 13 f' /^/V i yt; r " J / - r -... _ Extraction o f PFOS from /j / - v Serun\ jJ s *.** / - , * < ) ( J s ) U* *-> r / J - < ? , 2 ` / - ` !' 1 / L,' J tS * / J / C ~ f /* ,'' S / J <d j s t / j V c S 'i - f t 004301 J. :. yf *> s< C *' '** j Ion l'a ir S ta n d a rd C urves-il-N O O A (H um an S era - D eeatur S am ples) BEST COPY AVAILABLE Prep Daletx): 4/28/99 Study Number: (END11 Anaiyxl(.i): RWW Equipment Number: Sample Matrix: Human Sera Final Solvent itTN Number: MeOH / TN-A-2438 Method/Revision: ETS-8-4 0 Blank Fluid/ldcntitler: Rabbit Sera / TN-A-2391 Target Analyte(s): FC Mix (PFOS. PFOSA, PFOSAA, EtFOSE. PFOSEA. M556) FC Mix Sid Approx. 0.500 ppm: FC Mix Std Approx. 5.00 ppm: FC Mix Std Approx. 50.0 ppm: Surrogate Std Approx. 100 ppm: 99012-29-2 99012-29-1 99012-100 99012-3-24 Actual Concentrations of Standards in the FC Mix StM570, PFOS PFOSA PFOSAA EtFOSE Std Cone. Std Cone. Std Cone. Std Cone. ug/mL ug/mL ug/mL ug/mL 0.500 0.500 0.500 0.500 0.500 0.500 0.500 0.500 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 50.0 50.0 50.0 50.0 50.0 50.0 - 50.0' - 50.0 50.0 50.0 50.0 50.0 50.0 50.0 50.0 PFOSEA Std Cone. ug/mL- 0.500 0.500 5.00 5.00 5.00 50.0 50.0 50.0 50.0 M556 FC Mix Std Cone. Ain't Spiked ug/mL mL 0.500 0.010 0.500 0.020 5.00 0.005 5.00 0.010 5.00 0.020 50.0 0.005 . _ . j 0 ^ i - = " 0.010 50.0 0.015 50.0 0.020 All Final Volume mL 1.015 1.025 1.010 . J.01S 1.025 1.010 1.015 1.020 1.025 Calculated Concentrations of Standanis in the Sample Matrix. PFOS PFOSA PFOSAA EtFOSE Final Cone. ng/mL Final Cone. ng/mL Final Cone. Final Cone. ng/mL ng/mL 4.93 4.93 4.93 4.93 9.76 9.76 9.76 9.76 24.8 24.8 24.8 24.8 49.3 49.3 49.3 49.3 97.6 97.6 97.6 97.6 248 248 248 248 493 493 493 493 735 735 735 735 976 976 976 976 PFOSEA Final Cone. ng/mL 4.93 9.76 24.8 49.3 97.6 248 493 735 976 M5S6 Final Cone. ng/mL 4.93 9.76 24.8 49.3 97.6 248 493 735 976 Surrogate Std Cone. ug/mL 100 Surrogate Final Cone. ng/mL 500 All Am't Spiked mL 0005 Actual Concentrations of Standards in the FC Mix. PFOS PFOSA PFOSAA Std Cone. Std Cone. Std Cone. ug/mL ug/mL ug/mL MS 5.00 5.00 5.00 MSD 5.00 5.00 5.00 EtFOSE Std Cone. ug/mL 5.00 5.00 PFOSEA Std Cone. ug/mL 5.00 5.00 M556 Std Cone. ug/mL 5.00 5.00 FC Mix Am't Spiked mL 0.010 0.010 All Final Volume mL 2.011 2.011 Calculated Concentrations of Standards in the Rabbit Sera(.08 ml). PFOS PFOSA PFOSAA EtFOSE Final Cone. Final Cone. Final Cone. Final Cone. ng/rnL ng/mL ng/mL ng/mL 625.00 625.00 625.00 625.00 625.00 625.00 625.00 625.00 PFOSEA Final Cone. ng/mL 625.00 625.00 M556 Final Cone. ng/mL 625.00 625.00 Calculated Concentrations of Standards in Methanol(0.2 ml). PFOS PFOSA PFOSAA EtFOSE Final Cone. Final Cone. Final Cone. Final Cone. ng/mL ng/mL ng/mL ng/mL 250.00 250.00 250.00 250.00 250 00 250.00 250.00 250 00 PFOSEA Final Cone. ng/mL 250.00 250 00 MS56 Final Cone. ng/mL 250.00 250.00 GEN011 ion pair sheet.xls Surrogate Std Cone. ug/mL 100 Surrogate Final Cone. ng/mL 50 All Am't Spiked mL 0.001 Surrogate Std Cone. ug/mL 100 Surrogate Final Cone. ng/mL 200 All Am't Spiked mL OOOl 004302 FACT: DATA REVIEW SUMMARY FORM BEST COPY AVAILABLE D ate: __________ A nalyst: FACT Study Number Matrix Time Points t( t'W y a A * Analyte 4: Acceptable Linear Range: ^ -*i 7 - LOQ for this data set: 4 -f 7 Re-evaluated for different range? a J o Dilutions? Analyte 1: 7^T A w w i H M T m -- r P n o w 4 .T3-~ T T - EOQTSr dus data se t //J Re-evaluated fix different range? Analyte 2: ffio f Acceptable Linear Range: 4 - < a - LOQ for this data set 4 --IJ Re-evaluated for different range? /U Analyte 3: > "f a x T ____ Acceptable Linear Range: A 3 LOQ for ds data se t Re-evaluated for different range? j J a . 004303 i-ii fjyJb. guarir it/ Compound Summery Report Samp) L isr. C :\MASSLYNX\rats2 .PRO\Sample0B\043099al modified. Hon May 03 04:48:38 1999 Mathod C :\MA3SLYNX\rats2.PRO\MethDB\043099a Lear modified: Hon May 03 07:33:57 1999 Job Coda: Mon May 03 07:34:31 1999 Confound 1 : PFHS 1 Nama 1 v-n0990yl " 4 9 9 0 .: ) 4 j *i990V J 1 . 1- '#!,4 1 5' 9 9 'iiis .4 ;',790`jc. i<99rv 1 - . 4 5',990*id 4 ;4 099009 ' 1 4iU9901'j '>4 3 0 9 9 0 1 1 \ * 043099012 4 J `.'9901 3 4 . 99015. 99y 16 4 99017 :- .4 iC990!5 . . 4 9 9 0 L9 4 > 99'il*.* - l . 1 4 :9.9022 4 i->99023 4 >. >9024 t+ * t i ----~ *4 3 3 9 0 2 4 .4 3 0 9 9 2 "* :4099024 29 :43C99029 3<, >43099030 3: 043099031 3: 343099032 33 243099033 34 043099034 3* 3 4 3 0 9 9 0 3 5 0 343099036 37 343099037 3<i 34309903d 39 243099039 4*. 243099040 4*. 343299041 42 343099042 43 343099043 44 043099044 4 043099045 Samplallst Taxt G E N O U R8S04289-250 ppb G E N O U RBS4289-250 ppb HaOH Blank MeOH Blank G E NOU RBS4289-NBiank-l G E N O U RBS4289-SBlank-l G E N O U RBS04289-S ppb-1 GEN011 RBS04289-10 ppb-1 GEN011 RBS04289-25 ppb-1 G E N O U RB504289-50 ppb-1 G E N O U R8S04289-100 ppb-1 G E N O U RBS04289-250 ppb-1 G E N O U RBS04289-500 ppb-1 G E N O U RBS4289-750 ppb-1 MeOH Blme MOH Blank G E N O U RBS04289-HBlank-l GENOU, 9394 <0.09 mL) GENOU, 9395 <0.07 mL) GENOU, 9396 (0;08 mL) GENOU, 9397 <0.07 mL) GENOU, 9398 (0.07 mL) G E N O U RB504289-S0 ppb-1 MOH Blank G E N O U ABS4289-HBlank-l GENOU, 9399 <0.07 mL) GENOU, 9400 (0.07 mL) GENOU, 9401 (0.08 mL) GENOU, 9402 (0.08 mL) GENOU, 9403 (0.07 mL) G E N O U RBS04269-50 ppb-1 G E N O U R8S04289-250 ppb, MS G E N O U RBS04289-250 ppb, MSD G E N O U RBS04289-50 ppb-1 MeOH Blank G E N O U RBS04289-WBlan)e-2 G E N O U RBS04289-SBlank-2 G E N O U RBS04289-5 ppb-2 G E N O U RBS04289-10 ppb-2 G E N O U RBS04289-25 ppb-2 G E N O U RBS04289-S0 ppb-2 G E N O U RBS04289-100 ppb-2 G E N O U RBS04289-250 ppb-2 G E N O U RBS04289-S00 ppb-2 G E N O U RBS04289-7S0 ppb-2 BESTCOPY AVAILABLE ** 1 Typ Analyt* Analyte Analyte Analyte Analyte Analyte Standard Standard Standard Standard Standard Standard Standard Standard Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte QC Analyte Analyta Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte QC Analyte Analyte Analyte Standard Standard Standard Standard Standard Standard Standard Standard Std Cono AT 4.735 4.720 Area 473 521 Cone. riage %Oev 199.93 bb 220.14 bb 4.93 9.76 24.80 49.30 97.60 248.00 493.00 735.00 4.691 4.697 4.691 4.677 4.689 4.680 4.686 26 60 126 215 613 1107 1724 8.35 MM 23.01 MM 51.29 MM 89.51 bb 259.77 MM 470.97 MM 735.29 MM -14 -7 4 -8 S -4 0 4.689 4.677 4.682 4.686 4.685 49.30 4.705 -w. 4 . 6 4 4 - 216 537 636 . 1T7 70 139 --------- 50 89.73 MM 226.99 bb bb 73.01 m 27.18 t* i 56.93 m 18.61 M4 49.30 49.30 4.705 4.689 4.696 4.693 4.695 4.697 4.696 4.691 4.706 88 1188 479 300 527 130 679 651 143 35.06 m 505.91 KM 202.49 MM 125.96 bb 222.75 MM 52.97 MM 288.14 MM 276.12 MM 58.43 MM IS 7 19 4.93 9.76 24.80 49.30 97.60 248.00 493.00 735.00 4.699 4.702 4.706 4.697 4.694 4.684 4.701 35 60 127 243 543 1179 1774 12.27 MM 23.21 bb 51.86 MM 101.25 MM 229.85 MM 501.72 MM 756.56 MM 26 -6 5 4 -7 2 3 (w< e-'V ^ , v CftlcvA*^ ViOS ' U Orv<- 0A LAP fcuje Am alia 042498: R eview ed and q u a n tita te d by h o] 5 /3 /9 9 004304 S7?fcr Q u a n tify Compound Summary R ep o rt Sampi Lit: Last m odified: M othod: Last m odified: Job Cod C : \MASSLTNX\ra t s 2 . 9R 0\Sa*plDBVO 43O 99al Hon May 03 0 0 : 4 0 : 3 1999 C : \M A3SLTNX\cats2 . PR O \M th0B\043099a Mon May 03 0 7 : 3 3 : 5 7 1999 P rin te d Hon Hay 03 07:34:31 1999 Compound 2 . PFOS Name ;' rt' 4 >>>. 4 '* * '-4 4 i .4 4ji.i4ni. ; :4 43'* *90"9 4J'99GU. :43>`>9u 11 S43O99012 .J 43099013 .4 >43099014 )4 3099015 :i >43099016 1" 043099017 :*> 043099018 19 043099019 20 043099020 21 043099021 22 043099022 23 043099023 24 043099024 2V.4 3099025-- :e 543099026 1~ ;43099027 1<5 43099023 2 * 43^99029 !43..99->3i 4iv39031 * 4j 39*:32 4 j..990 23 34 .43099034 *43:99035 ir 4j :'99v36 ~ .4309903" :430 99C3c ? 143099039 4! 343099040 ;i 343099041 iZ .*43099042 42 343099043 44 043099044 45 043099045 Samplelist Test GENOli RBSU4289-250 ppb g e n o u rbs>';4289-25 ppb MeOH Blank MeOH Blank GCNOli RBSO4 20 9-WBUn*-l G E N O U RBS04289-SBlank-l G E N O U RBS04289-5 ppb-1 G E N O U RBS04289-10 ppb-1 G E N O U RBS04289-25 ppb-1 G E N O U RBSQ4239-50 ppb-1 G E N O U RBS04289-100 ppb-1 G E N O U RBS04289-2S0 ppb-1 G E N O U RBS04289-500 ppb-1 G E N O U ABS04289-750 ppb-1 MeOH Blank MeOH Blank G E N O U RB504289-WBlank-l GENOU, 9394 (0.09 mL) GENOU, 9395 (0.07 *L) GENOU, 9396 (0.08 LJ GENOU, 9397 (0.07 mL) GENOU, 9398 (0.07 mL) G E N O U RBSQ4289-SQ ppb-1 MeOH Blank G E N O U RBS04289-HBlank-l---GENOU, 9399 (0.07 mL) GENOU, 9400 (0.07 oL) GENOU, 9401 (0.08 mL) GENOU, 9402 (0.08 mL) GENOU, 9403 (0.07 mL) G E N O U RBS04289-50 ppb-1 G E N O U RBS04289-2SO ppb, HS G E N O U RBS04289-250 ppb, M5D G E N O U RBS04289-50 ppb-1 MeOH Blank G E N O U RBS04289-MBlank-2 G E N O U RBS04289-SBlank-2 G E N O U RBS04289-5 ppb-2 G E N O U RB504289-10 ppb-2 G E N O U RBS04289-25 ppb-2 G E N O U RBS04269-5 ppb-2 G E N O U RBS04289-100 ppb-2 G E N O U RBS04289-250 ppb-2 G E N O U RBS04289-500 ppb-2 G E N O U RBS04289-750 ppb-2 BESTCOPYAVAILABLE Bag 2 Type Analyte Analyte Analyte Analyte Analyte Analyte Standard Standard Standard Standard Standard Standard Standard Standard Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte OC Analyte Analyte Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte QC Analyte Analyte Analyte Standard Standard Standard Standard Standard Standard Standard Standard Std Cone 4.93 9.76 24.80 49.30 97.60 248.00 493.00 735.00 49.30 49.30 49.30 4.93 9.76 24.80 49.30 97.60 248.00 493.00 735.00 RT 5.283 5.267 5.254 5.237 5.244 5.238 5.249 5.259 5.250 S.255 5.281 5.240 5.246 5.250 5.233 5.256 5.251 5.256 5.239 5.244 5.240 5.245 5.248 5.246 5.238 5.2S6 5.250 5.248 5.251 5.252 5.265 5.245 5.253 5.249 Area 5641 6144 Cone. Flags %Oev 186.42 bb 196.10 bb 161 314 819 1551 2995 6950 12895 19202 4.71 bb 9.61 bb 25.76 bb 49.17 bb 95.39 bb 221.89 bbx 412.06 bbX 613.78 bbx -4 -2 4 0 -2 -U -16 -16 24 453 623 811 423-- 399 __ 1459 0.33 MK 14.06 bb 19.48 bb 25.51 bb X1.09 bb 12.33 bb 46.24 bb 347 671 489 1461 827 1591 7594 6928 1600 10.68 bb 21.04 bb 15.21 bb 46.32 bb 26.04 bb 50.46 bb 242.50 bb 221.18 bb 50.75 bb -6 2 3 176 319 765 1554 3135 6834 13256 19108 5.19 bb 9.77 bb 24.03 bb 49.28 bb 99.86 bb 218.18 bbX 423.61 bbx 610.79 bbX 5 0 -3 0 2 -12 -14 -17 EnW , , o ilv M LA A m lia 062 4 9 8 : Rv ie w e d and q u a n t i t a t e d b y h o ) 5 / 3 / 9 9 004305 i i Syten________________ Q u a n tify Compound Summary R ep o rt Samp La L i t ; C : \MASSLYHX\cats2 . F 8 O \5 a m p le0 B \0 4 3 0 9 9 a l L a st m o d ifie d : Mon May 03 0 6 : 4 8 : 3 0 1999 Mathod : C:\M A3SLYNX\rata2.PROVMathD\043099a L a s t m o d ifie d : Mon Hay 03 0 7 : 3 3 : 5 7 1999 Job Coda: P r in te d ; Mon May 03 0 7 : 3 4 : 3 1 1999 Co m po un d 3 PFDS Nama ; ,. Vim' * , **. .> .*>>... ;v '9'j'i4 4 : 90U * A 11.99006 f 41*;99009 AJ099010 0430990*1 '43099012 .3 1.-43099013 14 043099014 li >43099015 16 043099016 17 043099017 16 043099010 19 043099019 043099020 21 043099021 22 043099022 23 D43099023 24 043099024 2 5 ^ <3099023"^ 26 043099026 343099027 26 ,43099028 ?> 43099029 1 ,43'.-99030 i\ i3:99031 :. 43.:99032 4>*:99v33 1 43:.99034 43,99035 .:c .43099C36 j' U4309903*' JC 343099036 j9 343v 99j39 4, 043399040 41 043099041 42 C43C99042 43 343099043 44 043099044 45 043099045 Sampleliat Taxt J E N0U RBS04249-250 ppb 3ENU11 RBS'*4:99-250 ppb MeOH BlanK MeOH B U n k CEN01l RBS04289-UBlank-l G E N O U RBS4289-SBlank-l G E N O U RBSO4209-5 ppb-1 G E N O U RBS042B9-10 ppb-1 G E N O U RBS04289-25 ppb-1 G E N O U RBS04289-50 ppb-1 G E N O U RBS04289-100 ppb-1 G E N O U RBS04299-250 ppb-1 G E N O U RBS04289-S00 ppb-1 G E N O U RB504289-750 ppb-1 MaOH Blank MeOH Blank G E N O U RBS04289-WBlaak-l GENOU, 9394 (0.09 aL) GENOU, 9395 (0.07 u L ) GENOU, 9396 (0.08 aL) GENOU, 9397 (0.07 aL) GENOU, 9398 (0.07 aL) G E N O U RBS04289-50 ppb-1 MeOH Blank 'GENOU RBS04289-NBlank-l GENOU, 9399 (0.07 aL) GENOU, 9400 (0.07 aL) GENOU, 9401 (0.08 aL) GENOU, 9402 (0.08 aL) GENOU, 9403 (0.07 mL) G E N O U RB504289-S0 ppb-1 G E N O U RBS04289-250 ppb, MS GENOU RBS04289-250 ppb, MSD G E N O U RBS04289-50 ppb-1 MeOH Blank G E N O U R8S04289-WBlank-2 G E NOU RBS04289-SBlank-2 G E NOU RBS4289-5 ppb-2 G E NOU RBS04289-10 ppb-2 G E N O U RBS04289-2S ppb-2 G E N O U RBS04289-50 ppb-2 G E N O U RBS04289-100 ppb-2 G E N O U RBS04289-250 ppb-2 G E N O U RBS04289-500 ppb-2 G E N O U RBS04289-750 ppb-2 BESTCOPYAVAILABLE ! J, o o a < Typa Analyte Analyte Analyta Analyta Analyta Analyta Standard Standard Standard Standard Standard Standard Standard Standard Analyta Analyta Analyta Analyta Analyte Analyte Analyte Analyte OC Analyte Analyte Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte QC Analyte Analyte Analyte Standard Standard Standard Standard Standard Standard Standard Standard Std Cone AT 5.659 5.641 Area 12 23 Cone. Flags 65.74 bb 342.31 bb 4.93 9.76 24.80 49.30 97.60 248.00 493.00 735.00 49.30 ~ 49.30 49.30 S.SS3 S.590 S.644 5.654 5.626 5.632 10 8.72 bb 13 87.16 m 11 47.01 bb 19 249.53 bb 29 499.12 bb 34 632.03 MM 5.703 50 1030.72 bb 5.679 5.491 5.627 5.649 5.632 5.629 i.s- _____ 16 4 26 20 66 9 6 178.76 m 0.00 bb 428.38 bb bb 1440.50 bb 0.00 MM 0.00 KM 5.480 S.614 5.643 5.617 5.641 6 0.00 bb 23 344.15 bb 16 178.66 bb 22 328.33 bb 46 943.73 bb 5.647 5.639 23 341.84 bb 15 148.95 bb -65 77 -52 1 1 -14 -100 4.93 9.76 24.80 49.30 97.60 248.00 493.00 735.00 5.626 5.639 5.598 5.648 5.625 16 174.77 bbX 13 106.26 MM 23 355.64 Ml 28 473.47 MM 39 762.37 MM 255 9 43 -4 4 Pag 3 Am alia 062499: Raviawad and q u a n t ita ta d by h oj 5 /3 /9 9 004306 Quanti(y Calibration Report C al ib r a t io n : C: \MASflLYNX\rata2 . PK0\CurvaDB\O43O99a Laac m o d ifla d ; Hon May 03 0 7 : 3 4 : 0 3 1999 P rin tad : Mon May 03 0 7 : 3 9 : 4 4 1999 BESTCOPYA M BLE Compound I name: PFHS ...................... ........................... ' Coefficient o f Determination: 0.998313 Calibration curve: 2.33693 * x + 6.12110 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None 1.77e3 ? I i /- %Conc I T -14.4 0 .0 ------------------- -- ------ --------- :----------------- ^ --r -- ------------------------------------ Cone 100.0 200.0 300.0 400.0 50.0 600.0 700.0 A m alia 0 6 2 4 9 8 : R a v ia v a d and q u a n t i t a t a d b y ho) S / 3 / 9 9 004307 Q uantify C a lib ra tio n Raport Cal ibrar.io n : C : \HA3SLYNX\riu!.PR O \CurvaD B \043099a Lar. m o d ifie d : Mon May 0 ] 0 7 : 3 4 : 0 9 1099 P r in c a d Mon Kay 03 0 7 : 3 4 : 4 4 1999 BK C T Y AVAILABLE Compound 2 name: PFOS Coefficient o f Determination: 0.998987 Calibration curve: 31.2623 * x + 13.4094 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None 2.30e4 9*9 1 5.26 . /- %Conc T"'~' ~r"l' -16.9 0 .0 ---------------------------------------------------------,-- ---- ,,---,------------------------------------------Cone 100.0 200.0 300.0 400.0 500.0 600.0 700.0 062498: Raviwad and q u a n tita ta d by h o ) S /3 /9 8 004308 guanMfy Calibration Raport C a lib r a tio ft C :\M AM L YN X \rata2.PRO\CurvaOB\043099a L a s t r o e lifi* d : Mon Hay 03 0 7 : 3 4 : 0 3 1990 P n n ta d Mon May 0 3 0 7 : 3 9 : 4 4 1999 BESTCOPyAVAILABLE Compound 3 name: PFDS Coefficient o f Determination: 0.955785 Calibration curve: 0.0390723 * x + 9.30435 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None 39.1 ; Pag 3 /- %Conc -64.8 0 .0 ........................... ......... -- ,------ ----------------------- -- I---------------------------------------- Cone 100.0 200.0 300.0 400.0 500.0 600.0 700.0 Am alia 092498: R aviavad and q u a n tita ta d by h o) 9 /3 /9 9 004309 ' r / 7 ^ 7 ______________________ Quatf- ty Compound Summary R ap ort Sampl Li J t c : \M AS3LYNX\rats2 . P*0\SaiR pleO B \043099al U s e m o d ifie d : Mon May 03 0 6 : 4 9 : 3 1999 Hathod C: \H ASSLYNX\rata2 . PRO\M atb0B\043099* U s t m o d ifia d : Hon May 03 0 7 : 3 3 : 5 7 1999 Job Coda P r in ta d : Hon May 03 0 7 : 4 0 : 5 6 1999 Compound 1 : PFHS Kama : *4j*j99001 I ;4i**990ni i ,43^9*1)03 ^ /43u99uu4 i 4 )u9900S * >4JU990U6 ->43099007 4 -;4J'i99008 9 343099009 Im 34 3099010 1 ,4309901 1 i2 ,43099012 U ,43.,99013 N 43<.i)9014 >" .4 -99015 Ir ;3'-990i ; .43,99017 1 ,43v99U10 :3 43*99019 20 Ul 99020 !-43 >99021 22 >43)99022 23 34V.99023 24 :43?*99024 ri 2 42099026 27 >43099027 26 >43099029 29 >43099029 30 043099030 31 043099031 32 043099032 33 043099033 34 043099034 35 043099035 36 043099036 37 043099037 39 343099038 39 043099039 40 343099040 41 043099041 42 043099042 43 043099043 44 343099044 45 343099045 Samplaliat taxe G E N O U RBS04299-2S0 ppb G E N O U RBS04289-250 ppb MaOH Biank McOH filante G E N O U RBS04289-WBlank-l G E N O U RBS04289-$81ank-i G E N O U RBS04289-5 ppb-1 G E N O U RBS04289-10 ppb-1 G E N O U RBS04289-2S ppb-1 G E N O U R8S04289-50 ppb-1 G E N O U RBS04289-100 ppb-1 G E N O U RBS04289-250 ppb-1 G E N O U RBS04289-500 ppb-1 G E N O U RBSQ4289-75Q ppb-1 MeOH Biank MaOH Blantc G E N O U RBS04289-Blank-l GENOU, 9394 (0.09 mL) GENOU, 9395 <0.07 mL) GENOU, 9396 (0.0 a U GENOU, 9397 (0.07 al) GENOU, 9398 (0.07 &) G E N O U RBS04289-50 ppb-1 MaOH Blank *GEN011 RB504289-HBlank-l " GENOU, 9399 (0.07 mL) GENOU, 9400 (0.07 mL) GENOU, 9401 (0.08 aO.) GENOU, 9402 (0.08 mL) GENOU, 9403 (0.07 aL) G E N O U RBS04289-50 ppb-1 G E N O U RBS04289-250 ppb, MS G E N O U RBS04289-250 ppb, MSD G E N O U RBS04289-50 ppb-1 MaOH Blank G E N O U RBS04289-NBlank-2 G E N O U RBS04289-SBlank-2 G E N O U RBS04289-5 ppb-2 G E N O U RBS04289-10 ppb-2 G E N O U RBS04289-2S ppb-2 G E N O U R8S04289-50 ppb-2 G E N O U RBS04289-100 ppb-2 G E N O U RBS04289-25 ppb-2 G E N O U RBS04289-500 ppb-2 G E N O U RBS04289-750 ppb-2 BESTCOPYAVAILABLE typ* Analyta Analyta Analyca Analyca Analyta Analyta Standard Standard Standard Standard Standard Standard Standard Standard Analyta Analyta Analyta Analyta Analyta Analyta Analyta Analyta oc Analyta Analyta Analyta Analyta Analyta Analyta Analyta QC Analyta Analyta QC Analyta Analyta Analyta Standard Standard Standard Standard Standard Standard Standard Standard Std Cone 4.93 9.76 24.80 49.30 97.60 248.00 493.00 735.00 ___ 49.30 49.30 49.30 4.93 9.76 24.80 49.30 97.60 248.00 493.00 735.00 BT 4.735 4.720 4.691 4.697 4.691 4.677 4.689 4.680 4.686 4.689 4.677 4.682 4.686 4.685 4.705 4.644- 4.705 4.689 4.696 4.693 4.695 4.697 4.696 4.691 4.706 4.699 4.702 4.706 4.697 4.694 4.684 4.701 ATM 473 521 Cene. Plaga %Dev 199.93 bb 220.14 bb 26 60 126 215 613 1107 1724 8.35 MM 23.01 MM 51.29 MM 9.51 bb 259.77 MM 470.97 MM 735.29 MM -14 -7 4 -8 S -4 0 216 89.73 MM 537 226.99 bb 636.^. 26.51 bb 177 73.01 M4 70 27.1 m 139 56.93 MM - 50 18.61 MM 88 1188 479 300 527 130 679 651 143 35.08 MM 505.91 f*t 202.49 MM 125.96 bb 222.75 MM 52.97 MM 288.14 MM 276.12 MM 58.43 MM 15 7 19 35 60 127 243 543 1179 1774 12.27 MM 23.21 bb 51.86 MM 101.25 MM 229.S M M 501.72 MK 756.56 MM 26 -6 5 4 -7 2 3 Paga I Amalia 06249: Raviawed and q u a n tita te d by h oj 5 /3 /9 9 004310 s f<t Ift a s 9 I* C ft & ? ? 1ft O o O* to CJ K * VD I>U>*UO M* U IJ; I'J I l`Vl o OOOOOOOl AA j U U I u u u u;U U U - A A. J- 4. J lOOi o o o i? ip >o 0 o i I to * I, to to to o to to o o> 0 0 0 to to to to to> to to to o 0 0 0 ao to to to to ttoo ttoo o o o to to to c 41 to c 4t O , < U Ui U i u> w u Kl t J fJ t u>M* a g U i a u m o to a* 'J J t < f>Iv ISI -->r-J (I u>rJ . to a - .1 t J t<> U U O* O* UI * t J W W t i U u ' C 3 C i X >i.A A Xik U U u W2 E t O ^ ^ O ^ ^ t O t O O t O O i O t O t O O sDiOtO0 0 4 0 0 *o to tO o to to to to to to to to <c to tO to to to to to tO : c o - o o c c CO o c c 1W H o to O0itl<Xkui\l>-Ot04i -J tft Lit nnoncioQCit Z flO O O fO O O O O Z C IO flfC IQ O Z Z O fO fO fC IfO fZ Z O fM ggSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSS O O O O O O O O Q O X O O O O O O O O O O X O O O O O O O X X O O O O O O O O O O X X O O 'U 5O0S 5to0 6 (0>003 13 3 0) 9#SCD3 3O3D9CDV(A oSB n30 : tfl o U) o U UOUOA OU O) b O) (Of tOV M A0X0l A0 t0A0U 0) t0A 0* A* *0A0u U ) or Utou tUo Wt o Wt oW<0 I < f Jrg t*s> * M * M A A MMM *A MM * N M M NM * as >J s< u t i > 4 Kl Kl ) r I (A lA (A U M M (A (A (A I >0000000 o o kIAKIAKIAKiKi tlK*IKIK*I fifi aaa*av to to t.tO.iOt.L.l0.tt.O.t<.O.lt0.t.tO.t tO ttoit ol tlo t o o o o o o t o itMHViNHUtuiC ^_ < to O O O O O t to to a o a i B O 00 > tO tO tO tetO lO iO III > U* O O CO o _ os i >00 flOH *0V s i t i m icarcar cr& i i i m i i i i e s m i o or im w , Siau0otcS0Orciv0urotvi0oro*cO01ro*aU01o*oa0*Vc01-r < 9 X o 9 X i i 1 *JN N NM H* H $ii M Kl SS O SB SB O a a aro X vu* n oo fitti Kl Kl ft o a>M t(o tio f t Kl Kl U* ut oo *0 T a or ocr fCt n3-- Cit P"i n IIHI Ml ii gog*' 3 x" 3 x" ;h l K HK ( Ou rKz iod *rz< 3 ::g t*ot Xr toH i! ?& ?* SftSftSfStfitftSf!tft!ftf|tfSt'fStS Sft8 SftBftrftSftSftftfft 8S|f|t?SSSSSSSS???5 9 9 9 9 9 9 3 9 - f - f - f- f- -t-. ^ t-f~f-Hu**-t~f>9 9 9 3 9 9 9 9-'t~t~f~-K>ft aO aO Oa &O aO aO aO & srTKftKr krt*r<* *r<t<it<11<n<itf<tst f<t*f<tf<ti<t*r<r<r*t<t<t<ftaSfataftaSfaeOaftaftar>t<rt<ri<ft<ft<rT< aaaaaaa.fr Wu0OiwUO0OOfNO0lkO-OJUtOOeBK*O)<oOi t<OUo cocococoioiotoio NKl OuNUiNKUSMOt WUMtNHUNOOMOU to to u ui coiococototocococo MA( ABMUNd tNftfKtfIKi kIIOKf*JUMtOlKAJt F 1 IMUUHItMtAAoMtWUoKtO0fIKiA0n1OiK*OI0K^IOI UUUIlAtdOKOAI^itAO AKltO * oO Oo Oo Os Ou Oa O- iti Ua lAU tW AAAAU t NV( /KtAOJKAOIKStIOUKIBKAAIMUgKV*I m z 2 0 IH A guH tO U St U H H M S H lA tJ W H O U U U (A S H >J BAAUtjtuneoi CCOONIOto Id AK OtO*N* CBO r m ccrrccrrcirrccrr SOl Nt Ot OU ttOUNt Sl Ok OO Su li OU 0*H<4HtOH>i Ag AA HB AA BNMA HANK IHO HA AA AOBONUtOA *U)WA *MJ gV eerr ccrr tcrr Xa*Ttar ogr gu ag *U*SA* UtfUU* HWKHIWH N-4N0MA 0 AB HN tOI HA tAJMU OO SSSSSSi tMO KB)t(PA tKOl HO O U H OKItWOiUO UtOIUHHOMOSHt HA tgoAgOo AAgKt) e w AA Hg uOUAMIOWH MO IN0 cor-aaoc rrga carccrroor'oc xr 2S iit N3 N S 8 h 8 o r Quart M t y Compound Summary R ap ort Sample L is t Last m odified: M ethod L ast modi fia d : Job Coda C :\MASSLYNX\rata2.PRO\9ampleOB\043099el Hon May 03 06-48:39 189 C :\MASS1YHX\ rats2 .FRO\MethOB\043099a Hon May 03 0?:33:5? 1999 P rin te d Hon May 03 07:40:56 1999 Co m po un d 3: PPDS 1 Hama t ')4:ju39001 2 04 J099002 J 04)099003 4 043099004 i 04)099005 6 'J43099006 7 -.4 J'19D0 1 - `40990u8 9 `*4 3 v 9 9 y 0 9 lv .43-99010 U j4)u990U * `j43o'> 9'12 13 04)099013 14 U43099014 15 043099015 16 043099016 P 04)099017 L8 0 4 3 0 9 9 0 1 8 19 04)`:99019 21 343099020 21 v4Jv99021 :: v43*-99022 23 4)099023 v 2 4 tL,t'-.,l d 9 9 0 2 4 - ' 25 4 i 099025 26 v*!3`i9 9 0 2 2~ ->4 j v 9 9 0 2 '7 28 l-43';99028 29 ;4j .99029 30 343099030 31 ,43099031 32 V43099032 33 343099033 34 043099034 35 043099035 36 043099036 37 043099037 38 043099038 39 043099039 40 043099040 41 043099041 42 043099042 43 043099043 44 043099044 45 04309904S Saaplelist Taxt G E N O U RB504289-250 ppb G E N O U RBS04289-250 ppb MeOH Blank MeOH Blank G E N O U RBS04289-HBlank-l G E N O U RBS04289-SBlank-l G E N O U ABS04289-S ppb-1 G E N O U RBS04289-10 ppb-1 G E N O U RBS04289-2S ppb-1 G E N O U RBS04289-50 ppb-1 G E N O U R8S4289-100 ppb-1 G E N O U RBS04289-250 ppb-1 G E N O U RBS04289-500 ppb-1 G E N O U RBS04289-750 ppb-1 NOH Blank MaOH Blank G E N O U RBS0428 9-M8lank-1 GENOU, 9394 (0.09 aL) G ENOU, 939S (0.07 aL) G ENOU, 9396 tO.08 aL) G ENOU, 9397 |0.07 aL) GENOU, 9398 (0.07 aL) G E N O U RBS04289-50 ppb-1 - MaOH Blank - G E N O U RBS04289-MBlank-l GENOU, 9399 (0.07 aL) GENOU, 9400 (0.07 aL) GENOU, 9401 (0.08 aL) GENOU, 9402 (0.08 aL) GENOU, 9403 (0.07 aL) G E N O U RBS04289-50 ppb-1 G E N O U RB504289-2S0 ppb, HS G E N O U RBS04289-250 ppb, MSD G E N O U RBS04289-SO ppb-1 MeOH Blank G E N O U RBS04289-HBlank-2 G E N O U R8S04289-SBlank-2 G E N O U RBS04289-5 ppb-2 G E N O U RBS04289-10 ppb-2 G E N O U RBS04289-2S ppb-2 G E N O U RBS04289-S0 ppb-2 G E N O U RB504289-100 ppb-2 G E N O U RBS04289-2S0 ppb-2 G E N O U RBS04289-500 ppb-2 G E N O U RBS04289-750 ppb-2 BESTCOPYAVAILABLE Typa Analyte Analyte Analyte Analyte Analyte Analyte Standard Standard Standard Standard Standard Standard Standard Standard Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte oc Analyte Analyte Analyte Anelyte Analyte Analyte Analyte QC Analyte Analyte QC Analyte Analyte Analyte Standard Standard Standard Standard Standard Standard Standard Standard Std Cono RT 5.659 5.641 4.93 9.76 24.80 49.30 97.60 248.00 493.00 73S.00 5.553 5.590 5.644 5.654 5.626 5.632 5.703 49,30 5.679 5.491 5.627 5.649 5.632 5.629 "5.5*4 49.30 49.30 5.480 5.614 5.643 5.617 5.641 5.647 5.639 4.93 9.76 24.80 49.30 97.60 248.00 493.00 735.00 S. 626 S.639 5.598 5.646 5.625 Area 12 23 Cone. Flage %D#v 65.74 bb 342.31 bb 10 8.72 bb 13 87.16 MX 11 47.01 bb 19 249.53 bb 29 499.12 bb 34 632.03 MM 50 1030.72 bb 16 178.76 M4 4 0.00 bb 25 - 478.36 bb 20 262.40 bb <6 1440.50 bb 9 o.oo m 6 0.00 1M 6 0.00 bb 23 344.15 bb 16 178.66 bb 22 328.33 bb 46 943.73 bb 23 341.84 bb 15 148.95 bb -65 77 -52 1 1 -14 -100 16 174.77 bbX 13 106.26 MK 23 355.64 MM 28 473.47 MM 39 762.37 MM 255 9 43 -4 4 3 Am alia 062498: Raviawad and q u a n tita te d by h o ) 5 /3 /9 9 004312 Quantify Calibration Report C a n bra n o n C:\MASSLYNX\rata2. PRO \CurveDi\043099a L a st m o d if ie d : Mon May 03 0 7 : 4 0 : 3 9 1999 P rinted Mon May 03 0 7 : 4 0 : 5 1999 mwvMtm Compound 1 name: PFHS .............. .. Coefficient o f Determination: 0.998313 Calibration curve: 2.33693 * x + 6.12110 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None p9 1 I i /- %Conc 1-- 1 1 1 i ....... i 1iI -14.4 0 .0 ------------------------------------ _---------------- ---- -- n------1------------------------------------------ Cone 100.0 200.0 300.0 400.0 500.0 600.0 700.0 Amalia 062496: R eview ed and q u a n t i t a t e d by h o j 5 / 3 / 9 9 CG4313 Quantify Calibracin floport Cai ib ra tio n C : \MA33LYHX\rata2 . PR0\CurvaDS\OOO 99a L a s t m o d ifia d : Hon Hay 0 3 0 7 : 4 0 : 3 9 1 9 9 9 P r in ta d Hon Hay 03 0 7 : 4 0 : 5 9 1 9 9 9 K S raP M M IU ttE Compound 2 name: PFOS Coefficient o f Determination: 0.998238 Calibration curve: 26.7298 * x + 72.7186 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None 2 r /- %Conc T -3 3 .2 0.0 100.0 200.0 A m a lia 0 6 2 4 9 9 : R a v i wad and q u a n t i t Cad b y h o j 5 / 3 / 9 9 300.0 400.0 500.0 600.0 Cone 700.0 004314 M`. ' ; i - i M>:! : ` : La.-. f J . t J .rap- 'r. i . C: \.MASSLYNr.rat32 .PRONMethOBN043099a .adb Mon May iJ 07:33:5- 199: l: PFHS Mon May oj 07:53:34 1999 Ccmpouii'J Njmu : Interna'. Ref.: Ouanciiy Trace: Conc. s i Standards: User Ri /lue: User R-*: Factor: *r.*..r;r-- Window Factor: re*' - -j*..on Re1.:.'. Tune <nuns> : retention Time: T:s.s j :w *mmsi: ?*ut. ..*r. .r.or.: Keacvr.s Reaper.je Type: Response : Calibration Curves Polynomial Type: Point of Origin: Fit Weighting: gJcrs<Treme lerearfrion: Concentration Umts: Noise Peak-to-peak amplitude: Smooth Smoothing: Window size (scans): Number s i smooths: Smooching method: Sase. :r,ea Reoure peak tailing: Ra:se case.me maximum: Pea^ .lecaracion Craw vertical threshold: Cetect nouiders: Snou.cer threshold: Response Threshold Relative height: Absolute height: Relative area: Absolute area:- PFHS (None) TIC Conc. A 1.000000, Disabled 1.000000 2.000 4.407, enabled 0.000, Disabled 0.584 Nearest External Areas Linur Excluda 1/X None 206 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 AmL 0 ( . M ______L A C 0 5 o > l f i 004315 M-' M.iM. i . . . :<*<i: 'Jumji'.'ifi-i Hr in *i: C :\MASSLYNX\rats2 .PR0\MethD8\043099a .mdb Hon Hay oj 07:33:57 1999. 2 : PFOS Hon May 03 07:53:34 1999 lasip'.m. I N.me inrr m .,. it .: Juan'. :/ Trace: 'J-m :. .: standards: User hk Value : User PeaK Factor: Integra*: e Window Factor: Pea* Leeet ion fletei.r ; .f. '"ime (minsi : ke .-it. ketention Time: r.fl**.* a . :. : w m:nsi : ... * .> : PFOS (None) TIC Conc. A 1.000000, Disabled 1.000000 2.000 5.195, Enabled 3.000, Disabled 0.390 Nearest kesp'.r.A- 'VP*: Resp:.:. External Areas Calicrat .on Curves Polynomial Type: P o m e of Origin: Tit Weighting: fat- Beene farma&lon: Concentration Linear Exclude 1/X Nne Units: Noise Pear.-co-peak amplitude: Smooth Smoothing: Window size (scans): Number of smooths: Smoothing method: Disabled 3 2 B aselines Join valley threshold: Reduce peak tailing: Raise case line maximum: 2 0 .0 0 50.00 5.00 Pea/: J e t s : a :to r . Ira* vart.ra. threshold: i*e*.ei-'. sr.tuloers: Sr.ru.ser threshold: 10.00 Disabled 40.00 Response Threshold Relative height: Absolute height: Relative area: Absolute area: 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled ] BEST COPY AVAILABLE----- A iyJi OLlHU iAC- os/l/w 004316 :oP' .s H t t n f }! C:\MASSLNX\rats2.PRO\MethDB\043099a.adb l: Mon May oj 07:33:57 19991 3: PFDS Mon May 03 07:53:34 1999 tn t*tt juari' Jtuncurds: 1 U ser Hi V alu : {i User Reek factor: Integrate Window Factor t Peak Location Rr.r.t::n Time imins): Pela'. :/ Retention Time Time mina: ^ig .i; : PFOS INonel TIC Conc. A 1l..000000000000 Disabled 2 .0 0 0 5.573 Enabled 0.000 Disabled 0.226 Nearest 1 i J I J Resp-ir.s*' Type: Resptr..**: Calibration Curves Polynomial Type: Point z i Origin: fit Weignting: 'A&cr^'-Tmisfuiation: Concentration Units: Noise Peak-tc-peak amplitude: Smooth Smoothing: Window size (scans): Number of smooths: Smoothing method: Basel me s J o m va. :y threshold: Reduce peak tailing: Raise Caseline maximum: Peak Sparation Detect s.-.culders: She-.ser threshold: Rspense Tr.resnold Relative heignt: Absolute heignt: Relative area: Absolute area: External Areas Linear Exclude 1/X None 80 Disabled 3 2 20.00 SO. 00 S.OO 10.00 Disabled 40.00 1.50 Disabled 0.00 Disabled 2.00 Disabled 0.00 Disabled IESTCOPY AVAILABLE A*L__ u m i IA<\ m l o i / n - ' le J 004317 Q u a n tity Compound Summary R ep o rt QEM-Oil Hunan S e r a / Q u a l i t a t i v Compound C haek Sample Lit: C: \MASSLfNX\rACT-l .FR0\fl^lSB\OSO3b Laat modified: Men May 03 10:01:10 199 Mathod: C:\MASSLYNX\rACT-l.PRO\MethDS\030399b Laat modified: Tua May 04 11:04:31 1999 job Coda: Printed: Tua May 04 11:19:20 1999 Compound 1 : P O M Hana 8anplll*t Taxt 1 0S0399006 KaON Blank 2 050399007 MaOK Blank 3 0S0399008 G E N O U RBS04289-WBlank-l 4 050399009 G E N O U RBS04289-SBlank-l 5 050399010 G E N O U R8S04239-5 ppb-1 6 050399011 G E N O U RBS04289-1O ppb-1 7 050399012 G E N O U RBS04289-2S ppb-1 3 050399013 G E N O U RBS04289-SO ppb-1 9 050399014 G E N O U RB504289-100 ppb-1 10 050399015 MeOH Blank 11 050399016 MaOH Blank 12 0S0399017 G E N O U RBS04289-WBlank-1 13 050399018 GENOU. 9394 (0.09 mL) 14 050399019 GENOU. 9395 (0.07 mL) IS 050399020 GENOU. 9396 (0.08 mL) 16 050399021 GENOU, 9397 (0.07 mL) 17 050399022 GENOU. 9398 (0.07 mL) 18 050399023 G E N O U RBS04289-S0 ppb-1 19 050399024 MaOH Blank 20 050399025 G E N O U RBS04289-WBlank-l a 850399026 ~GEH0U, 9399 (0.07 mL) 22 050399027 GENOU. 9400 (0.07 mL) 23 0S0399028 GENOU. 9401 (0.08 mL) 24 050399029 GENOU, 9402 (0.08 mL) 2S 050399030 GENOU, 9403 (0.07 m U 26 050399031 G E N O U RBS04289-S0 ppb-1 27 050399032 G E N O U RBS04289-250 ppb, HS 28 050399033 G E N O U R8S04289-250 ppb, HSD 29 050399034 G E N O U RBS04289-50 ppb-1 30 050399035 MaOH Blank 31 050399036 G E N O U RBS04289-WBlank-2 32 050399037 G E N O U RBS04289-SBlank-2 33 050399038 G E N O U RBS04289-S ppb-2 34 050399039 G E N O U RBS04289-10 ppb-2 3S 050399040 G E N O U RBS04289-2S ppb-2 36 050399041 G E N O U RBS04289-5O ppb-2 37 050399042 G E N O U RBS04289-100 ppb-2 BESTCOPyAVAILABLE Typa Analyta Analyte Analyta Analyta Standard Standard Standard Standard Standard Analyta Analyta Analyta Analyta Analyta Analyta Analyta Analyta QC Analyta Analyta Analyta Analyta Analyta Analyta Analyta QC Analyta Analyta OC Analyta Analyta Analyta Standard Standard Standard Standard Standard td Cone 4.93 9.76 24.80 49.30 97.60 49.30 --- 49.30 49.30 4.93 9.76 24.80 49.30 97.60 RT 5.112 5.102 S.023 S.074 5.030 5.039 5.016 5.041 5.029 5.097 5.046 S.019 5.012 S.019 5.019 S.020 5.042 5.039 5.013 5.022 5.034 5.013 5.023 5.017 5.020 5.043 5.120 5.034 5.045 S.OSO 5.030 5.014 5.034 5.020 -- Area Di. . 29 1 22 1 34 1 38 1 61 1 50 1 45 1 68 1 86 1 28 1 39 1 98 1 100 1 113 1 137 1 124 85 1 42 --- n 203 127 111 168 as 130 101 S3 20 30 61 38 47 49 56 86 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 Cne. Plaga %Dev 0.00 MM 0.00 MK 0.00 MM 0.00 MM 43.68 MM 786 12.23 KM 25 0.00 KM 100 65.90 MM 34 120.18 MM 23 0.00 KM 0.00 KM 155.38 bb 162.84 bb 202.02 MM 273.88 bb 233.37 bb 117.39 MM 138 0.00 MM 134.42 bb 473.43 bb 243.87 bb 195.93 bb 365.67 bb 116.98 bb 251.12 bb 166.53 bb 21.61 KM 0.00 MM 0.00 MM 43.72 KM 0.00 MM 2.51 MM 7.88 MM 28.58 MM 119.72 MM 137 -56 -100 -74 -68 -42 23 1 p 9 M e t -/oree w )< b im Soup 020199: Q uan titatad and p rin ta d b y drb 0 5 /0 4 /9 9 C0431S Q u a n tify Conpound lu ia u r y R eport QBN-011 Human S e r e / Q u a l i t a t i v e Compound C heck M p l L i t : C:\NAS8LYNX\rACT-l.PRO\SaMpleDB\0S0399b IrAflt M o d i f i e d : Mon May 03 16:01:10 1999 Method: C :\MASOLYMX\PACT-1. PRO\MethDB\05039b Lest Modified: Tue Mey 04 11:06:31 1999 Job Code: Printed: Tue Mey 04 11:19:20 1999 Canpound 2: M463 Mene 1 050399006 2 050399007 3 050399008 4 0S0399009 5 050399010 6 050399011 7 050399012 8 050399013 9 05Q39914 10 050399015 11 050399016 12 050399017 13 050399018 14 050399019 IS 050399020 16 050399021 17 050399022 18 050399023 19 050399024 20 050399025 2-fostatale 22 050399027 23 050399028 24 050399029 2S 050399030 26 050399031 27 050399032 28 050399033 29 050399034 30 050399035 31 050399036 32 050399037 33 050399038 34 050399039 35 050399040 36 050399041 37 050399042 8enplellst Text MeOH Blenk MeOH Blenk G E N O U RBS04289-WBlenk-l G E N O U RBS04289-SBlank-l G E N O U RBS04289-5 ppb-1 G E N O U RBS04289-10 ppb-1 G E N O U RBS04289-25 ppb-1 G E N O U RBS04289-50 ppb-1 G E N O U RBS04289-1QQ ppb-1 MeOH Blenk MeOH Blenk G E N O U RBS04289-WBlank-l GENOU. 9394 (0.09 aL) GENOU. 9395 (0.07 aL) GEN011. 9396 (0.08 aL) GENOU. 9397 (0.07 aL) GENOU. 9398 (0.07 aL) G E N O U RBS04289-50 ppb-1 MeOH Blenk GEN011 RBS04289-WBlaak-l l a w n , 3s <o.o7 mu GENOU. 9400 (0.07 aL) GENOU. 9401 (0.08 aL) GENOU. 9402 (0.08 aL) GENOU. 9403 (0.07 aL) G E N O U RBS04289-50 ppb-1 G E N O U RBS04289-250 ppb. MS G E N O U RBS04289-250 ppb. MSO G E N O U RBS04289-50 ppb-1 MeOH Blenk G E N O U RBS04289-WBlank-2 G E N O U RBS04289-SBlenk-2 G E N O U RBS04289-5 ppb-2 G E N O U RBS04289-10 ppb-2 G E N O U RBS04289-25 ppb-2 G E N O U RBS04289-50 ppb-2 G E N O U RBS04289-100 ppb-2 .--. BESTCOPYAVAILABLE Type Anelyee Analyte Anelyee Analyte Standard Standard Standard Standard Standard Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte QC Analyte Analyte Analyte Standard Standard Standard Standard Standard Std Cone 4.93 9.76 24.80 49.30 97.60 49.30 ---- 49.30 49.30 4.93 9.76 24.80 49.30 97.60 RT 5.259 5.279 5.285 5.259 5.289 mi 5.280 5.291 5.275 5.254 -- 5.256 5.287 Area Dl. . Cone. Plage 21 1 20 1 22 1 34 1 48 1 20 1 18 1 20 1 47 1 47 1 17 1 17 1 MMZ MMX MMX MMX MMX MMX MMX MMX MMX MMX MMX MMX thUryi. U<_ Pepe 2 oup 020199: Q uantitated end p rin ted by drb 0 3 /0 4 /9 9 004319 KST COPYAVAILABLE Q u a n tify Compound Sum tary R ep ort 0 0 1 - 0 1 1 Minean S a r a / Q u a l i t a t i v a Compound Cheek lanpla Lit: C: \MAJSLYKX\rACT-l .PRO\SMpleM\0S0399b Last nodifiad: Moo May 03 16:01:10 1999 Mathod: C:\MA6SLYMXVFACT-l.rRO\MeehDb\0S0399b Last Modified: Tua May 04 11:04:31 1999 Job Coda: Prineed: Tua May 04 11:19:20 1999 Compound 3: M313 Naaa 1 050399006 * 050399007 3 050399008 4 050399009 S 050399010 6 050399011 7 050399012 8 050399013 9 050399014 10 050399015 11 050399016 12 050399017 13 050399018 14 050399019 15 050399020 16 050399021 17 050399022 18 050399023 19 050399024 20 050399025 'll? 22 050399027 23 050399028 24 050399029 25 050399030 26 050399031 27 050399032 28 050399033 29 050399034 30 050399035 31 0S0399036 32 050399037 33 050399038 34 050399039 35 050399040 36 050399041 37 050399042 mpl.list t u t MaOH Blank MaOH Blank G E N O U RBS04289'WBlank-l G E N O U RBS04289-SBlank-l G E N O U RBS04289-5 ppb-1 G E N O U RBS04289-10 ppb-1 G E N O U RBS04289-25 ppb-1 G E N O U RBS04289-50 ppb-1 G E N O U RBS04289-100 ppb-1 MaOH Blank MaOH Blank G E N O U RBS04289-WBlank-1 GENOU. 9394 (0.09 mL) GENOU. 9395 (0.07 *L) GENOU. 9396 (0.08 *L) GENOU. 9397 (0.07 mL) GENOU. 9398 (0.07 aL) G E N O U RBS04289-50 ppb-1 KaOK Blank G E N O U RBS04289-WBlank-l 9399 (0.07 mL) GENOU, 9400 (0.07 aL) GENOU. 9401 (0.08 mL) GENOU. 9402 (0.08 aL) GENOU. 9403 (0.07 aL) G E N O U RBS04289-50 ppb-1 G E N O U RBS04289-250 ppb, NS G E N O U RBS04289-250 ppb. MSD G E N O U RBS04289-50 ppb-1 MaOH Blank G E N O U RBS04289-WBlank-2 G E N O U RBS04289-SBlank-2 G E N O U RBS04289-S ppb-2 G E N O U RBS04289-10 ppb-2 G E N O U RBS04289 -25 ppb-2 G E N O U RBS04289-50 ppb-2 G E N O U RBS04289-100 ppb-2 D i> Hg 3 c cj ( < ^ I c f ___________________________ Typa Analyta Analyte Analyta Analyta Standard Standard Standard Standard Standard Analyta Analyta Analyta Analyta Analyta Analyta Analyta Analyta oc Analyta Analyta Analyta Analyt Analyt. Analyta Analyta QC Analyta Analyta QC Analyta Analyta Analyta Standard Standard Standard Standard Standard Std Cene 4.93 9.76 24.80 49.30 97.60 49.30 49.30 49.30 4.93 9.76 24.80 49.30 97.60 Area 01.. Cone. Plaga hOav Q .u iila k < *. c t a t a d a )^ Ut Soup 020199: Q uantItatad and p rla ta d by drb 0 3 /0 4 /9 9 004320 BESTCOPVAVAILABLE Q u 4 A tiiy Compound f u m u r y R apore OEN-Oll Human S a r a / Q u a l i t a t i v Compound Cback lampi List : C: \MASSLYMX\FACT-1 .FR0\EamplOB\05O399b Last isodifid: MOO May 03 16:01:10 1999 Mstbod: C:\KASSLna\rACT-l.FHO\MatbDS\050399b Last modified: Tua May 04 11:06:91 1999 Job Cods: Printad: Tu May 04 11:19:30 1999 Compound 4 : surr 9 Wtm Saa^lolist Taxt 1 050399006 MeOH Blank 2 050399007 HeOH Blank 3 050399008 G E N O U ABS04289-WBlank-l 4 050399009 G E N O U RBS04289-SBlank-l 5 050399010 G E N O U RBS4289-5 ppb-1 6 050399011 G E N O U RBS04289-10 ppb-1 7 050399012 G E N O U RBS04289-25 ppb-1 8 050399013 G E N O U RBS04289-S0 ppb-1 9 050399014 G E N O U RBS04289-100 ppb-1 10 050399015 MeOK Blank 11 050399016 KeOH Blank 12 050399017 G E N O U RBS04289-WBlank-l 13 050399018 GENOU, 9394 (0.09 *L> 14 050399019 GENOU, 939S (0.07 mL) IS 050399020 GENOU, 9396 (0.08 mL) 16 050399021 GENOU. 9397 (0.07 mL) 17 050399022 GENOU, 9398 (0.07 mL) 18 050399023 G E N O U RBS04289-50 ppb-1 19 050399024 itoOK Blank 20 050399025 G E N O U RBS04289-WBlank-l -31/ 05039*026--QCM011, 9399 (0.07 mL) 22 050399027 GENOU. 9400 (0.07 mL) 23 050399028 GENOU, 9401 (0.08 mL) 24 050399029 GENOU, 9402 (0.08 mL) 2S 050399030 GENOU, 9403 (0.07 mL) 26 050399031 G E N O U RBS04289-50 ppb-1 27 050399032 G E N O U RBS04289-250 ppb, MS 28 050399033 G E N O U RBS04289-2S0 ppb. MSS 29 050399034 G E N O U R8S04289-50 ppb-1 30 050399035 MOK Blank 31 050399036 G E N O U RBS04289-WBlank-2 32 050399037 G E N O U RBS04289-SBlank-2 33 050399038 G E N O U RBS04289-S ppb-2 34 050399039 G E N O U RBS04289-10 ppb-2 35 050399040 G E N O U RBS04289-2S ppb-2 36 050399041 G E N O U RBS04289-50 ppb-2 37 050399042 G E N O U RBS04289-100 ppb-2 ~ Typ Analyt Analye Analyt Analyt Standard Standard Standard Standard Standard Analyt Analyt Analyt Analyt Analyt Analyt Analyt Analyt QC Analyt Analyt ' - - Analyt Analyt Analyt Analyt Analyt QC Analyt ' Analyt QC Analyt Analyt Analyt Standard Standard Standard Standard Standard ed Cene 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 XT Area Di Cone. Fl aff %Dv 5.016 5.008 5.022 5.002 S.009 5.OOS 5.022 1624 1839 1769 1875 1791 1535 1891 1 1 1 1 1 1 1 0.81 bb 0.91 bb 0.88 bb 0.93 bb 0.89 bb 0.76 bb 0.94 bb -19 -9 -12 -7 -11 -24 -6 5.010 5.012 5.004 5.012 5.012 5.012 5.006 1893 3937 4584 4072 4269 3633 1782 1 1 1 1 1 1 __ 1 0.94 bb 1.96 bb 2.28 bb 2.03 bb 2.12 bb L.81 bb 0.89 bb 5.032 5.006 5.015 4.998 5.006 5.016 5.010 5.013 5.007 2179 - --- 4258- - 4844 5032 4395 7774 1979 4326 3993 2442 1 1 1 1 1 1 1 1 1 1 1.08 bb 2.12 bb 2.41 bb 2.50 bb 2.19 bb 3.87 bb 0.98 bb 2.15 bb 1.99 bb 1.21 bb 5.026 5.008 5.014 5.023 5.006 5.027 5.013 1896 2227 2203 2162 2241 2449 2194 1 1 1 1 1 1 1 0.94 bb 1.11 bb 1.10 bb 1.07 bb 1.11 bb 1.22 bb 1.09 bb -6 96 128 103 112 81 -11 8 112 141 150 119 287 -2 115 99 21 6 11 10 7 11 22 9 hoi tritrej L A t D S I, d s } * 0 oup 030199: Q u an titt* and p rio ta d by drb 09 /0 4 /9 9 C04321 Method Report Method file: Last modified: Compound: Printed: C:\MASSLYNX\PACT~l.PRO\MethDB\050399b.ndb Tue May 04 11:06:51 1999 1: PAA Tu# May 04 14:11:29 1999 Compound Ma m : Internal Ref.: Quantify Trece: Cone, of Stend*rdf: User nr Velue: User Peek Pector: Integrate Window factor: PQAA (None) TIC Cone. A 1.000000. Dieebled 1.000000 2 .0 0 0 Retention Tine (ins) Relative Retention Tine: Tine Window (nine): Peek Selection: 4.976. Cnebled 0.000. Dieebled 0.421 Neereet Response Type: Response: external Areas Polynomial Type: Point of Origin: Pit Weighting: Axis Transformation: Linear Include 1/X Mone Units: Peak-to-peak amplitude: 230 Smoothing: Window sire (scans): Number of smooths: Smoothing method: Disabled 3 2 Join valley threshold: Reduce peak tailing: Raise baseline amximum: 20.00 100.00 0.00 Draw vertical threshold: Detect shoulders: Shoulder threshold: 10.00 Disabled 40.00 Relative height: Absolute height: Relative area: Absolute area: oo CO N 1.50. Disabled 0.00, Disabled 2.00, Disabled 60.00, Enabled Soup i S 1AC. slsfol p*0* * BEST GOPITA V M U B IE I i i Method Report Method f i l e : L ett M odified: Compound: Printed: C: \MASSLYNX\FACT~1. PRO\M ethDB\0S0399b.*db Tue Key 04 1 1 :0 6 :5 1 1999 2: M463 Tue Nay 04 Compound Naaci Internal Ref.: Quantify Trace: Cone, of Standards: User RP Value: User Peak factor: Integrate Window factor: M469 (Mona) TIC Cone. A 1.000000, Disabled 1.000000 2.000 Retention Tiat (ins) t Relative Retention Tine: Time Window (ins): Peak Selection: 5.302, Enabled 0.000, Disabled 0.188 Nearest Response Type: Response: Polynomial Type: Point of Origin: Pit Weighting: Axis Transformation: External Areas Linear Exclude 1/X Hone Units: Peak-to-peak amplitude: 114 Smoothing: window site (scans): Humber of smooths: Smoothing method: Disabled 3 2 Join valley threshold: Reduce peak tailing: Raise baseline maximum: 20.00 100.00 Q.QQ Draw vertical threshold: Detect shoulders: Shoulder threshold: 10.00 Disabled 40.00 Relative height: Absolute height: Relative area: Absolute area: 6 & CO to CO 1.50, Disabled 0.00, Disabled 2.00, Disabled 80.00, Enabled b lo w it i IA l 0i l o s h `1 P*g 2 OESTCOPY AVAILABLE I- l I Method Report Method f i l e : Last M odified: Compound: Printed: C :\MASSLYNX\FACT-1.PRO\HethDB\0S0399b.mdb Tue May 04 1 1 :0 6 :5 1 1999 3: M513 Tue May 04 14:11:29 1999 Compound Naai: Internal Ref.: Quantify Trace: Cone, of Standards: User RP Value: User Peak Factor: Integrate Window Factor: MSI3 (None) TIC .Cone. A 1.000000, Disabled 1.000000 2.000 Retention Tine (nine): Relative Retention Tine: Tine Window (nins): Peak Selection: 6.324, Enabled 0.000, Disabled 0.724 Nearest Response Type: Response: External Areas Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation; Linear Exclude 1/X None Units: Peak-to-peak amplitude: 114 Smoothing: Window sise (scans); Humber of smooths: Smoothing method: Disabled 3 2 Join valley threshold: Reduce peak tailing: Raise baseline maximum: Draw vertical threshold: Detect shoulders: Shoulder threshold: 20.00 100.00 0.00 10.00 Disabled 40.00 Relative height: Absolute hgight: Relative area: Absolute area: ^ 6 CO to 1.50, Disabled 0.00, Disabled 2.00, Disabled 60.00, Enabled S o u p -- Z l V i j ___ I Tt A, it l A t . OS'! o i l Pge 3 BEST COPY AVAILABLE I I i v K- i z -- -c -x ) Method Report Method f i l e : L est M odified: Compound: Printed: C:\KASSLYNX\fACT-1.PRO\M ethDB\050399b.mdb Tue Mey 04 1 1 :0 6 :5 1 1999 4: surr Tue Mey 04 14:11:29 1999 Compound Name: Internel Ref.: Quantify Trece: Cone, of Stenderds: User RF Velue: User Peek Fector: Zntegrete Window Fector: surr (Nonel TIC Fixed 1.000000, Disabled 1.000000 2.000 Retention Tie (ins): Relative Retention Tise: Tiac Window (mins): Peek Selection: 4.925, Enebled 0.000, Disabled 0.146 Nearest Response Type: Response: External Areas Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Linear Exclude 1/E None Units: Peak-to-peak amplitude: 114 Smoothing: Window sise (scans): Humber of smooths: Smoothing method: Disabled 3 2 Join valley threshold: Reduce peak tailing: Raise baseline maximum: 20.00 100.00 0.00 Draw vertical threshold: Detect shoulders: Shoulder threshold: 10.00 Disabled 40.00 Relative height: Absolute height: Relative area: Absolute area: 6^ 5 CO ro C/l 1.50, Disabled 0.00, Disabled 2.00, Disabled 80.00, Enabled Ut. DSls/i Pge 4 b es t c o py m i m e i; { I S' m m nrtMOH I 2222222222222222222IH2222222M22222 jinr^HHrr.ooto(or>rHoHioooiAe^cs0r*><~ir>^r>*w o<N9'tninnHe(ieneiA4p|HHooai>tiAiA0(ano4niA PUO O O O * O t 0 i B O O O O O O O O r ' O^ O O O O O O H * 4 9 oO \O O O t f o W o t U > ` mh H O 49n>a^9<>oMOtrO<f4noArar>'AootHMenanr4^*rt>eHn0%9i^M9i<fD<t4arif4>H4 *i r4rtN ! * rtrlrlHHHHHHH Orl0 91 m h r* rr*or*rH*oe HnH i H<IIm i n i A i A 9 M r h h M < M n N W N H A n i 4 0 N 9 p < t r i H O H H 9 W Kf(999in09900H90iri9p99<0inn999WWW9 H H H r4 0 O 0 O 0 H r H H H H H H 0 H H M H i> t^i-l0 0 0 0 H H H 0 0 0 0 0 n r-oa on <o<) 9 9 h n9n n0tro9oftoo i l M 1U13M13h13h9) b l M I M M UUUUa<44tUlPUiMiltU NSNS'd'OOD ....5.=..7 . 5 1 1 2 2 1l H H H H H r 4 r 4 H dM44 U '-^ U U U h U ttU h *> u 9H3bUU9fb13h*0 > >t >*>*>*% h U o ss 9 H MH H >H 9*9 C9<919 I iiiiiii lliis^i ilss8 H lIo o oeem! Sr4 ro>or *o oo 9or * oOmOOt Of > e m unm HH A i ....... . i i t O 0 0 0 0 0 0 9 ) 9 0 0 0 0 0 9 9 9 9 1 O) 9) O) O)0 O) 0 ***-, * -* w , - , o w * o 9 a a M NNNN <9(9999f9 f9M OOOOO 0- 0. 0. 9- 0. 0.. 0_ 0 0 ) 0 0 0 0 0 0 0 0 OOOOOOO W a Vt d U n WV n i Q JJqt(Jj <gQti^9i |io9nn^n9nn^n'nn^n~nHg">ll g|^n 9^9^9 9^H^V igngi fg)gi (-lgA Vg)g )gMgV )gVg| igA >9f-t * H r4 2 2 e 5 * = C oP<orloHoHoHoHoHa pHpHpHoHpHoHoHpHpHopBl ! oM o*4ot-4ot-iow-tow-to9 2222222222a22a5B12888222222222232 U U U U D IS O O O O U S D p O O O O O O O O S Q U O O O O O hOOr4Nn9VI WhO0OH 9n<Oh0AOr4Nn9lAOha0 9>'0po'0pr'r-r*r'r'r-r-r'r-r' oooaOOOOOOOOOOO 0 0%0 0 O O' 9 O' 0 O' 0) 010 0 0 _ OOOOOOOOOOOOOOOO 000000000000000 nnnnnnnnrtrtffirtrtrt O' 0 0 O' O' O' O' O' 0 0 O' 9 O' O' 9 O' ilrtrt rt rt ri n pi r o o o ^ rtn OinOinOinOifO0OifOliOntOniOniOniO/nOniOntOfi tfVO(OntOntOnOniOftOinOioOiiOnmOmtOAmOi/OtOntOnm OOOOOOOOOOOOOOO - OOOOOOOOOOOOOOOO 99hO0Or4r<n9intehO9 n CO CM n o<o* Soup 020199 : Quantitt! and prlatad by drb 09/05/99 Q u a n tify Compound Sum eary R ap ort GEN-011 Human S a r a / Q u a l i t a t i v a Compound C hock SZ srm ampia Lit: C:\MASSLmX\rACT-l.PR0\SaNeleOB\O5O399c Last modified: Mon Nay 03 11:43:03 1999 Method : C :\MA88LYNX\PACT-1. PRO\Meth0R\OSO399e Last modified: Nad May OS 09:39:53 1999 Job Code : Printed: Wad Nay 03 10:03:17 1999 / iM w C p o u n d 3 : PPOSAR Hama Samplalist Text 1 05039900 MeOH Blank 2 050399044 MeOH Blank 3 050399045 G E N O U RBS04289-WBlank-l 4 050399046 G E N O U RBS04289-SBlank-l 5 050399047 G E N O U RBS04289-5 ppb-1 6 050399040 G E N O U RBS04289-10 ppb-1 7 050399049 G E N O U RBS04289-25 ppb-1 8 050399050 G E N O U RSS04289-50 ppb-1 9 050399051 G E N O U RBS04289-100 ppb-1 10 050399052 MeOH Blank 11 050399053 MeOH Blank 12 050399054 G E N O U RBS04289-N81ank-1 13 050399055 GENOU. 9394 (0.09 mL) 14 050399056 GENOU. 9395 (0.07 mL) 15 050399057 GENOU, 9396 (0.08 mL) 16 050399058 GENOU. 9397 (0.07 mL) 17 050399059 GENOU. 9398 (0.07 mL) 18 050399060 G E N O U RBS04289-50 ppb-1 19 050399061 MeOH Blank 20 050399062 G E N O U RBS04289-WBlank-l 21 050399063 GENOU. 9399 (0.07 mL) 22 050399064 GENOU, 9400 (0.07 mL) -- 2 * OlHomOBS "CBm D U . 9401 (0.08 mL) 24 050399066 GENOU, 9402 (0.08 mL) 25 0S0399067 GENOU, 9403 (0.07 mL) 26 050399068 G E N O U RBS04289-S0 ppb-1 27 050399069 G E N O U RBS04289-250 ppb, MS 28 050399070 G E N O U RBS04289-250 ppb. MSO 29 050399071 G E N O U RBS04289-50 ppb-1 30 050399072 MeOH Blank 31 050399073 G E N O U RBS04289-VBlank-2 32 0S0399074 G E N O U RBS042S9-SBlank-2 33 050399075 G E N O U RBS04289-5 ppb-2 34 0S0399076 G E N O U RBS04289-10 ppb-2 35 050399077 G E N O U RBS04289-25 ppb-2 36 050399078 G E N O U RBS04289-50 ppb-2 37 050399079 G E N O U RBS04289-100 ppb-2 Type Analyte Analyte Analyte Analyte Standard Standard Standard Standard Standard Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte QC Analyte Analyte Analyte Standard Standard StandardStandard Standard Std Cone RT Area 01.. Coac. Piaga hOev 4.93 9.76 24.80 49.30 97.60 5.649 5.688 5.690 5.647 5.691 55 1 4.14 MM 118 1 10.42 bb 277 1 26.28 bb 517 1 50.30 bb 948 1 93.37 bb -16 7 6 2 -4 5.648 5.687 5.658 49.30 5.688 29 1 33 1 29 1 1.54 MM 1.94 MK 1.56 MM 515 1 50.13 bb 2 _______ 14- 1 0.02 MM 49.30 49.30 5.645 5.687 5.645 5.644 5.664 5.647 36 651 2217 2102 529 31 1 2.23 MM 1 63.72 bb 1 220.16 bb 1 208.65 bb 1 51.46 bb 1 1.80 MM 4.93 9.76 24.80 49.30 97.60 5.646 5.690 5.645 5.649 5.675 62 1 4.87 KM 109 1 9.57 bb 273 1 25.91 bb 539 1 52.51 bb 969 1 95.40 MM 29 4 -1 -2 4 7 -2 Q u l i l c l l i,x, c L i a a entrd. Ut D s ld s fc *9 2 o u p 02 0 1 9 9 : Q u w t l t a t a d and p r i n t ! toy drto 0 5 /0 5 / 9 9 C 0 4 3 o r w Q u a n tify Compound lu i-- a r y R ep o rt GEM-011 Human f o r a / Q u a l i t a t i v a Compound C hock z z best copy m fampia Lit: C; \NMBLnot\rACr-l .PRO\SaemleDB\0S0399c Last nodifiad: Mon May 03 1<:43:03 1999 Method: C:\MRJiLYNX\FACT-l.rilO\MeehDa\050Jf9c Laat modified: Mod May 03 09:33:35 1999 Job Code: Printed: Mod May 03 10:03:17 1999 iu is ^ ^ Compound 3: M370 a Marne Bamplellat Tant i 050399043 MeOH Blank 2 050399044 MeOH Blank 3 05039904S G E N O U RBS04289~MBlank-l 4 050399046 G E N O U RBS04289-SBlank-l 5 050399047 G E N O U RBS04289-5 ppb-1 6 050399048 G E N O U RBS04289-10 ppb-1 7 050399049 G E N O U RBS04289-2S ppb-1 8 050399050 G E N O U RBS04289-50 ppb-1 9 050399051 G E N O U RBS04289-100 ppb-1 10 0503990S2 MeOH Blank 11 0503990S3 MeOH Blank 12 050399054 G E N O U RBS04289-MBlank-l 13 0503990S5 GENOU. 9394 (0.09 mL) 14 050399056 GENOU. 9395 (0.07 mL) IS 050399057 GENOU. 9396 (0.08 mL) 14 050399058 GENOU. 9397 (0.07 mL) 17 050399059 GENOU. 9398 (0.07 mL) 18 050399060 G E N O U RBS04289-50 ppb-1 19 050399061 MeOH Blank 20 050399062 G E N O U RBS04289-WBlank-l Ql<099999863 ''GENOU, 9399 (0.07 mL) 22 050399064 GENOU. 9400 (0.07 mL) 23 050399065 GENOU. 9401 (0.08 mL) 24 050399066 GENOU. 9402 (0.08 mL) 25 050399067 GENOU. 9403 (0.07 mL) 24 050399068 G E N O U RBS04289-50 ppb-1 27 050399069 G E N O U RBS04289-250 ppb. MS 28 050399070 G E N O U RBS04289-2S0 ppb. KSD 29 050399071 G E N O U RBS04289-5O ppb-1 30 050399072 MeOH Blank 31 050399073 G E N O U RBS04289-WBlank-2 32 050399074 G E N O U RBS04289-SBlank-2 33 050399075 G E N O U RBS04289-5 ppb-2 34 0S0399076 G E N O U RBS04289-10 ppb-2 35 050399077 G E N O U RBS04289-2S ppb-2 34 050399078 G E N O U RBS04289-SO ppb-2 37 050399079 G E N O U RBS04289-100 ppb-2 Typ Analyte Analyte Analyte Analyte Standard Standard Standard Standard Standard Analyte Analyte Analyte Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte Analyte Analyte Analyte Analyte Analyte QC Analyte Analyte QC Analyte Analyte Analyte Standard Standard Standard Standard Standard ltd Cone 4.93 9.76 24.80 49.30 97.60 49.30 ----mi 49.30 49.30 4.93 9.76 24.80 49.30 97.60 Area Di ^ Cone. Plaga %Dev QucJ.'kJirt ciak 0\ )ltn LAc, 3 Soup 020199: Q u a n tita ted and p r in te d b y drb 0 3 /0 3 /9 9 004328 QuA n e lf y C o ^ o u n d l u a u c y Rapor e QSN-011 Human S a r a / Q u a l i t a t i v a Compound C baek ZZ Iampia Lit: C:\MAfl8LYNX\rACT-l.Pk0\SaaplaOB\0S0399e Late nodiflad: Mon Kay 03 10:43:03 1999 Haehod: C:\NA4SLYia\rACT-l.RRO\Natk0B\OSO399e Last nodlflad: wad May OS 09:S3:SS 1999 Job Coda: rlatsd: Wad Kay OS 10:03:17 1999 BESTCOPYAVAILABLE^ ) / / Compound 4: K5SC Wma Bamplalist Taxe l 050399043 MaOH Blank 2 050399044 MnOH Blank 2 0S039904S G E N O U RBS04289-WBlank-l 4 050399046 G E N O U RBS04289-SBlank-l S 050399047 G E N O U RBS04289-5 ppb-1 6 050399048 G E N O U RBS04289-10 ppb-1 7 050399049 G E N O U RBS04289-25 ppb-1 8 0S039905O G E N O U R8S04289-50 ppb-1 9 050399051 G E N O U RBS04289-100 ppb-1 10 050399052 MaOH Blank 11 050399053 MaOH Blank 12 050399054 G E N O U RBS04289-WBlank-l 13 050399055 GENOU. 9394 (0.09 mL) 14 050399056 GENOU. 9395 (0.07 mL) 1S 050399057 GENOU. 9396 (0.08 mL) 16 050399058 GENOU. 9397 (0.07 mL) 17 050399059 GENOU. 9398 (0.07 mL) 18 050399060 G E N O U RBS042S9-50 ppb-1 19 050399061 MaOH Blank 20 050399062 G E N O U RBS04289-WBlaiik-l 21 050399063 GENOU. 9399 (0.07 mL) 22 050399064 GENOU. 9400 (0.07 mL) -2> 5jEUaS-US*M011, 9401 (0.08 mL) 24 050399066 GENOU. 9402 (0.08 mL) 25 050399067 GENOU. 9403 (0.07 mL) 26 050399068 G E N O U RBS042B9-S0 ppb-1 27 050399069 G E N O U RBS04289-250 ppb. MS 28 050399070 GEN011 RBS04289-250 ppb. MSD 29 050399071 G E N O U RBS04289-S0 ppb-1 30 050399072 MaOH Blank 31 050399073 G E N O U RBS04289-WBlank-2 32 050399074 G E N O U RBS04289-SBlank-2 33 050399075 G E N O U RB504289-S Ppb-2 34 050399076 G E N O U RBS04289-10 ppb-2 35 050399077 G E N O U RBS04289-2S ppb-2 36 050399078 G E N O U RBS04289-50 ppb-2 37 050399079 G E N O U RBS042B9-100 ppb-2 ... . Typa Analyta Analyta Analyta Analyta Standard Standard Standard Standard Standard Analyta Analyta Analyta Analyta Analyta Analyta Analyta Analyta QC Analyta Analyta Analyta Analyta ~ _ Analyta Analyta Analyta QC Analyta Analyta QC Analyta Analyta Analyta Standard Standard Standard Standard Standard Std Cne 4.93 9.76 24.80 49.30 97.60 49.30 -- -. 49.30 49.30 4.93 9.76 24.80 49.30 97.60 RT 5.588 5.540 5.544 5.543 5.545 5.543 =* - -- 5.542 5.498 5.497 5.552 5.585 5.543 5.542 5.544 5.529 Araa 01.. 41 1 81 1 223 1 388 1 726 1 339 1 --- 358 2121 1985 389 1 1 1 1 48 1 72 1 180 1 403 1 661 1 Cono. Flags %Dav 4.33 MM 9.82 MM 29.23 bb 51.68 bb 97.90 bb -12 1 18 S 0 45.08 bb -9 47.61 KM 288.47 bb 269.87 bb 51.86 bb -3 5 5.29 MK 8.52 KM 23.27 bb 53.72 bb 89.03 NM 7 -13 -6 9 -9 Qu)/4cW cAt\ LAC Raga 4 oup 03019*: Q u u tlt t d u d p r ln ta d b y drb O S/O S/t 004329 Q u a n tify Compound l u n u x y R ep o rt GEN-011 Ku m a l a r a / Q u a l i t a t i v Compound C bck ZZ Saopl Lit: C:\MAJ8LnaVrACr-l.Pft0\SaHplaOB\0S0399e Last nodlfid: Men May 03 10:43:03 1999 Method: C:\MAlBLYVX\FACT-l.PIIONMathSB\0S0399e Last Modified: Wed May 09 09:53:35 1999 Job Cod: Printed: wed May 05 10:03:17 1999 Confound 5: surr Man amplellst Txt 1 050399043 MeOH Blank 2 050399044 KeOK Blank 1 050399045 G E N O U RBS04289-WBlank-l 4 050399046 G E N O U RBS04289-SSlank-l 5 050399047 G E N O U RBS04289-S ppb-1 6 050399048 G E N O U RBS04289-10 ppb-1 7 050399049 G E N O U RBS04289-25 ppb-1 8 050399050 G E N O U RBS04289-50 ppb-1 9 050399051 G E N O U RBS04289-100 ppb-1 10 050399052 MeOH Blank 11 050399053 MeOH Blank 12 050399054 G E N O U RBS04289-WBlank-l 13 050399055 GENOU, 9394 (0.09 mL) 14 050399056 GENOU, 9395 (0.07 mL) 15 050399057 GENOU, 9396 <0.08 mL) 16 050399058 GENOU, 9397 (0.07 mL) 17 050399059 GENOU, 9398 <0.07 mL) 18 050399060 G E N O U RBS04289-50 ppb-1 19 050399061 MOH Blank 20 050399062 G E N O U RB542B9-WBlank-l 21 050399063 GENOU, 9399 (0.07 mL) 22 050399064 GENOU, 9400 (0.07 m L) aa - -GENOU, 9401 (0.08 mL) 24 050399066 GENOU, 9402 (0.08 mL) 25 050399067 GENOU, 9403 (0.07 mL) 26 050399068 G E N O U RBS04289-50 ppb-1 27 050399069 G E N O U RBS04289-250 ppb, MS 28 050399070 G E N O U RBS04289-250 ppb, MSB 29 050399071 G E N O U RBS04289-50 ppb-1 30 050399072 KaOH Blank 31 050399073 G E N O U RBS04289-WBlaak-2 32 050399074 G E N O U RBS04289-SBlank-2 33 050399075 G E N O U RBS04289-5 ppb-2 34 050399076 G E N O U RBS04289-10 ppb-2 35 050399077 G E N O U RBS04289-2S ppb-2 36 050399078 G E N O U RBS04289-50 ppb-2 37 050399079 G E N O U RBS04289-100 ppb-2 BEST COPY AVAILABLE Type Analyte Analyte Analyte Analyt Standard Standard Standard Standard Standard Analyt Analyt Analyt Analyt Analyt Analyt Analyt Analyt OC Analyt Analyt Analyt Analyt Analyt Analyt Analyt OC Analyt Analyt QC Analyt Analyt Analyt Standard Standard Standard Standard Standard Std Cena KT Arsa Dl.. 1.00 1.00 1.00 1.00 1.00 4.994 4.998 4.997 5.035 4.996 4.996 4.999 2048 2299 2055 2153 2000 1683 1988 1 1 1 1 1 1 1 1.00 4.995 4.999 4.992 4.994 4.990 4.997 4.993 1986 4144 4751 4225 4496 3691 1738 4.996 4.995 . 4.991 -- - -- f?* 4.994 4.994 1.00 4.996 4.992 4.992 1.00 4.998 ---- 1964 4095 4606 <m4196 8708 2756 4008 4109 2293 1.00 1.00 1.00 1.00 1.00 4.997 4.992 4.994 4.995 4.992 4.997 4.983 1928 2064 2028 1931 2202 2260 2071 1 1 1 1 1 1 1 ~-- 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 Cone. Flaps SDmr 1.01 bb 1.13 bb 1.01 bb 1.06 bb 0.98 bb 0.83 bb 0.98 bb 1 13 1 6 2 -17 -2 0.98 bb 2.03 bb 2.33 bb 2.07 bb 2.21 bb 1.81 bb 0.85 bb -- 0.96 bb 2.01 bb 2.26 bb 2.41 bb 2.06 bb 4.27 bb 1.35 bb 1.97 bb 2.02 bb 1.13 bb 0.95 bb 1.01 bb 1.00 bb 0.95 bb 1.08 bb 1.11 bb 1.02 bb -2 103 133 107 121 81 -15 -4 101 126 141 106 327 35 97 102 13 -5 1 0 -5 8 11 2 0 ioup 020199: Q u an tltatad and p rin ted by drb 0 5 /0 5 /9 9 04330 Q uantity C a lib ra tio n Raport 0 0 1 -0 1 1 Hunan f o r a / Q u a l i t a t i v o Compound Chock XX Calibration: C:\MUJLYllX\rACT-l.fKO\CurvoOS\050399c Last nodi M a d : Nod Nay OS 09:Sf:13 1999 frlntodt Nod Nay OS 09:S:44 1999 BSTOPAVAft.ABtE 9ago 1 oup 010199: Q uantitated and p ria ta d by drb 0 5 /0 5 /9 004331 Q uantify C a lib ra tio n Raport OXM-Oll Hunan farm / Q u a l i t a t i v CnaRMimid C hack XX Calibration: C:\MRJOLtltt\rJuCT-i.PRO\CurvaOk\OS0299c Last nodi Clad: Wad May OS 09:90:13 1999 Priatad: Wad May OS 09:50:44 1999 BESTCOPYAVAILABLE '9 a floup 0 2 0 1 9 9 : Q u a a t lt a t a d and p r in t a d toy d rb 0 3 / 0 5 / 9 * 004332 Q uantify C a lib ra tio n Raport QKM-OU Hunan i a r a / O u a l l t a t i v a Compound C hock IX Calibration: C:\lttJ9LYKX\7ACT-l.W0\Curvo0b\0S0399c Last aodlflod: Mod Kay OS 09:5f:12 19S9 Printod: Mod May OS 09:SS:44 19S9 BESTCOPTAWiLABLE ^9 3 oup 030199: Quantltatod and prlntod by drb 05/0S/99 004333 Quantity Calibration Haport anr-011 m a n Sara / Qualitativ Ccapouad O u e k ZZ Calibration: C:\NMLY)tX\r&CT-l.ttONCurvaa\0S0399c Laat xlifiad: Wnd May OS 09:34:12 1999 ?rlatd: Wad Nay OS 09:59:44 1999 B E S T C O P T ffl l E ou p 020199: Q u a n tita ta d and p r in te d b y drb OS/OS/99 004334 Quantify Calibration apart OCH-Oll Hunan Sara / Qualitativo Compound Chaek II Calibration: C: \MfLYia\rACT-l.PftO\CurvnOB\OS03f Se Laat aodifiad: Wad May OS 00:50:13 ISSO Printad: Wad May OS OS:SO:44 1SSS BESTCOPYAVAILABLE ** S oup 0201SS: Q uantitatad and p rin ta d by drb 0S/0S/SS 004335 Method file: Lest Modified: Compound: Printed: C: \MASSLYNX\FACT-1. PRO\MethDB\050399c.rtb Wed Hay 05 09:55:55 1999 1: PFOSA 10:02:08 1999 m 0 1 CoMiound Ni m : Internal Ref.: Quantify Trace: Cone, of Standards: User ft? Value: User Peak Factor: Integrate Window factor: PFOSA (None) TIC Cone. A 1.000000. Oisabled 1.000000 2.000 Retention Time (sins): Relative Retention Time: Time Window (mins): Peak Selection: i.OiS, Enabled 0.000. Disabled 0.298 Nearest Response Type: Response: external Areas Polynomial Typai Point of Origin: Pit Weighting: Axis Transformation: Limar Exclude 1/X None Units: Peak-to-peak amplitude: Smoothing: Window size (scans): Number of smooths: Smoothing method: 230 Disabled 3 2 Join valley threshold: Reduce peak tailing: M i c e baseline maximum: 20.00 100.00 0.00 Drew vertical threshold: Detect shoulders: Shoulder threshold: 10.00 Disabled 40.00 Relstive height: Absolute height: Relstive area: Absolute ares: 1.50. Disabled 0 .00. oisabled 2.00. Disabled 80.00. Enabled C>0 | 9 9 V 1* \ -*r l C b s k s /9 9 P*g* 1 Method Report Method file: Lest Modified: Compound* Printed: C: \MASSLYMX\PACT-1. PRO\MethDB\0S0399c .adb Mod May OS 09:55:55 1999 2 1 PPOSAA Wed May OS 10:02:08 1999 Compound Mue: Internal Ref.: Quantify Trace: Cone, of Standards: User RP Value: User Peak factor: Integrate Window factor: PF05AA (Mone) TIC Cone. A 1.000000, Disabled 1.000000 2.000 'Sbuj) 020)9 Retention Tis (eins): Relative Retention Tisw: T i Window (nins) ; 5.650, tnabled 0.000, Disabled 0.424 I Peak Selection: Nearest Response type: Response: External Areas Polynomial Type: Point of Origin: Pit Weighting: Axis Trans formation: Linear Exclude 1/X None Units: Peak'to-peak amplitude: 114 Smoothing: Window sise (scans): Nuater of smooths: Smoothing method: Disabled 3 2 Join valley threshold: Reduce peak tailing: Raise baseline maxis: Draw vertical threshold: Detect shoulders: Shoulder threshold: 20.00 100.00 0.00 10.00 Disabled 40.00 Relative height: Absolute height: Relative area: Absolute area: 1.50, Disabled 0.00, Disabled 2.00, Disabled 80.00, Enabled 004337 l * lAC osjc^lv i i l F*g* 2 C* Q, Method R eport Method t i l t s Last modified: Coapound: Printed: C:\MASSLYNX\PACT-l.PRO\MethDB\050399c.mdb Wed May 05 09:5S:55 1999 5: surr Wed May 05 10:02:09 1999 Compound Nan: Internal Ref.: Quantify Trace: Cone, of Standards: User RP Value: User Peak Factor: Integrate Window Factor: surr (None) TIC Fixed 1.000000. Disabled 1.000000 2.000 Retention Tise (mins): Relative Retention Tisw: Time Window (mins): Peak Selection: 4.913. Enabled 0.000, Disabled 0.037 Nearest Response Type: Response: External Areas Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Linear Exclude 1/X None Unit*: Peak-to-peak amplitude: 114 Smoothing: Window sise (scans): Member of smooths: Smoothing method: Disabled 3 2 Join valley threshold: Reduce peak tailing: Raise baseline maximum: 20.00 100.00 0.00 Draw vertical threshold: Detect shoulders: Shoulder threshold: 10.00 Disabled 40.00 004338 Relative height: Absolute height: Relative area: Absolute area: 1.50, Disabled 0.00, Disabled 2.00, Disabled 80.00, Enabled Y 1 lA L n z l s /f? Page S en I 3M Environmental Laboratory Note to File 3M E T & S S L a b o ra to ry S tu d y N o. C B N 0 11 Associated Study N um ber: ?dAA M fr3- d -- <L "V " I c r^ c tiU ? 5. P i ^ 2 , C * A U .e * l 2 it NO M S lV M Sl^S U i r * T ^ s< S t JL * - U Ls ih fc>____p s A - Vj ' ^ t y o ____ U V ^ J y U - . - L e t' t% rf< a } Q > b F Q A _____ d i i ..> iTt/^vyj____ o s 2 i z p & 3 2 ________ e c f . / j j j c i c f > V K f f V S f l __ / i f M J e -c te st) J ^ y ^ ^ c U ^ i h t-t r f t ^ L J U 9 ^ f* * 3 Z f T 40 .h^yO___f J z r h o c l ^ i s 4 . ( jjJ e c ti^ w J L C t w ^ < ' -t~ V LL ftp o - p cUjttcJhtd I/ ^ w - ^ ___________________________ ^ 1 l / < c - K i L h . . J k / x x \ d j i -- . . ___________________ Recorded By: f ct i Date 004339 Q u a n tify Compound turns*r y R e p o r t R at U r in H athOd D e v e lo p m e n t. SKI Sample Lit: 9 :\FACT-1.PR0\8apleDa\OSO399b Last Modifiad: Mon Hay 03 1 4 : 0 1 : 1 0 1999 Hathod: 9 :\FACT-1.PRO\HethDB\0S0399b Last isodifiad: Tua Hay 04 11:04:31 1999 Job Coda: Printed: r n Hay 21 11:54:44 1999 Compound 1: PQAA Name l 050399006 2 050399007 3 050399008 4 050399009 S 050399010 6 050399011 7 050399012 8 050399013 9 050399014 10 050399015 11 050399016 12 050399017 13 050399018 14 050399019 15 050399020 16 050399021 17 050399022 18 050399023 19 OS0399024 20 050399025 21 050399026 22 050399027 24 050399029 25 050399030 26 050399031 27 050399032 28 050399033 29 050399034 30 050399035 31 050399036 32 050399037 33 050399038 34 050399039 35 050399040 36 050399041 37 0S0399Q42 Saapleliat Test MsOH Blank MaOH Blank GENll ABS04289-WBlank-l G E N O U RBS04289-SBlank-l G E N O U RBS042B9-S ppb-1 G E N O U RBS04289-10 ppb-1 G E N O U RBSQ4289-25 ppb-1 G E N O U RBS04289-50 ppb-1 G E N O U RB504289-100 ppb-1 HaOH Blank MaOH Blank G E N O U RBSQ4289-NBlank-l GENOU/ 9394 (0.09 L> G ENOU/ 9395 (0.07 b L) G ENOU/ 9396 (0.08 b L) G ENOU, 9397 (0.07 b L) GE N O U , 939% (0.07 aOA G E N O U R8504289-S0 ppb-1 MaOH Blank G E N O U RBS04289-WBlank-l G E N O U , 9399 (0.07 b L) G E N O U , 9400 (0.07 b L) G E N O U , 9401 (0.08 b L) --GENOU/ 9402 (0.08 aL) G E N O U , 9403 (0.07 b L) G E N O U RBS04289-50 ppb-1 G E N O U R8S04289-250 ppb, MS G E N O U RBS04289-250 ppb, MSO G E N O U RBS04289-50 ppb-1 HaOH Blank G E N O U RBS04289-WBlank-2 G E N O U RBS04289-SBlank-2 G E N O U RBS04289-5 ppb-2 G E N O U RBS04289-10 ppb-2 G E N O U RBS04289-2S ppb-2 G E N O U RBS04289-50 ppb-2 G E N O U RBS04289-100 ppb-2 BESTCOPYAVAILABLE 9 1 ' -- Typa Analyta Analyta Analyta Analyta Standard Standard Standard Standard Standard Analyta Analyta Analyta Analyta Analyta Analyta Analyta Analyta QC Analyta Analyta Analyta Analyta Analyta Analyta Analyta QC Analyta Analyta QC Analyta Analyta Analyta Standard Standard Standard Standard Standard Std Cone 4.93 9.76 24.80 49.30 97.60 49.30 49.30 49.30 4.93 9.76 24.80 49.30 97.60 RT 5.112 5.102 5.023 5.074 5.030 5.039 S.016 5.041 5.029 5.097 Aras 29 22 34 38 61 50 45 68 86 28 5.046 5.019 5.012 5.019 5.019 3.020 S.042 r 39 98 100 113 137 124 85 5.039 5.043 5.022 5.034 5.013 5.023 5.017 5.020 5.043 5.120 5.034 5.045 5.050 5.030 5.014 5.034 5.020 42 91 -- 203 127 111 168 85 130 101 53 20 30 61 38 47 49 56 86 Response 29.033 22.095 33.979 38.037 60.565 50.106 44.822 67.951 85.999 27.584 39.225 97.701 100.182 113.209 137.099 123.630 A5.069 42.226 90.731 203.445 127.121 111.183 167.617 84.935 129.533 101.407 53.226 19.637 29.864 60.576 37.984 46.876 48.660 55.542 85.844 Cone. Flags %Dav 0.00 MM 0.00 MM 0.00 MM 0.00 MM 30.62 MM 521 0.00 MM -100 0.00 MH -100 67.77 MM 37 158.54 MM 62 0.00 MM 0.00 MM 217.39 bb 229.87 bb 295.39 MM 415.54 bb 347.80 bb 153.86 MM 212 0.00 MK 182.34 bb 749.22 bb 365.36 bb 285.20 bb 569.03 bb 153.19 bb 377.49 bb 236.03 bb 0.00 MM 0.00 MM 0.00 MM 30.68 M K 0.00 MMX 0.00 MMX 0.00 MMX 5.36 MMX 157.76 MMX 211 -100 -100 -100 -100 -89 62 soup 020199::q u a n tita ta d and p rin ta d by 004340 Q u a n tify Compound S u m a r y JU p o r t Hat U rin Hthod D avalopa i n t , SIS 3aa*l Liat : 9 :\FACT-1. PRO\flMplOB\050399b Laat aodifld: Mon May 03 15:01:10 1999 Mthod: B:\rACT-l.?R0\MthDB\OSO399b Laat odifid: Tu May 04 11:05:51 1999 Job Cod: Pnntd: Pri May 21 11:54:44 1999 Compound 2 : M4 53 Nana L 050399006 2 050399007 3 050399008 4 050399009 5 050399010 6 050399011 7 050399012 8 050399013 9 050399014 10 050399015 11 050399016 12 0S0399017 13 050399018 14 050399019 15 050399020 16 050399021 1? 050399022 18 50399023 19 050399024 20 050399025 21 050399026 22 050399027 "23^50^99021 24 050399029 25 050399030 26 050399031 27 050399032 28 050399033 29 050399034 30 050399035 31 050399036 32 050399037 33 050399038 34 050399039 35 050399040 36 050399041 37 050399042 Saaplllat Txt McOH Blank MaOH Blank G E N O U RBS042B9-WBlank-l G E N O U RBS04289-3Blank-l G E N O U RBS04289-S ppb-1 G E N O U RBS04289-10 ppb-1 G E N O U RBS04289-25 ppb-1 G E N O U RBS04289-50 ppb-1 G E N O U RBS04289-100 ppb-1 MaOH Blank KOH Blank G E N O U RBS04289-HBlank-l GENOU, 9394 (0.09 aL) GENOU, 9395 (0.07 aL) GENOU, 9396 (0.08 aL) GENOU, 9397 (0.07 aL) GENOU, 9398 (0.07 aL) G E N O U RBS04289-5Q ppb-1 NOK Blank G E N O U RBS04289-tfBlank-1 GENOU, 9399 (0.07 aL) GENOU, 9400 (0.07 aL) * GENOU, 9401 (0.08 aL) GENOU, 9402 (0.08 aL) GENOU, 9403 (0.07 aL) G E N O U RBS04289-50 ppb-1 G E N O U RB504289-250 ppb, MS G E N O U RB504289-250 ppb, MSD G E N O U RBS04289-50 ppb-1 MOH Blank . G E N O U RBS04289-WBlank-2 G E N O U RBS04289-SBlank-2 G E N O U RBS04289-5 ppb-2 G E N O U RBS04289-10 ppb-2 G E N O U RBS04289-25 ppb-2 G E N O U RB504289-50 ppb-2 G E N O U RB504289-100 ppb-2 BESTcopy AVAILABLE Typa Std Cne RT Ara Raapon Gene. Fia An.lyt. Analyta Analyta Analyta Standard 4.93 Standard 9.76 Standard 24.80 Standard 49.30 Standard 97.60 Analyta Analyta Analyta Analyta 5.259 21 20.984 MMI Anlyt 5.279 20 20.379 MMX Analyta S.28$ 22 22.269 MMX Analyt 5.259 34 34.007 MMX Aoncalyta $.21 49.30 48 48.086 MMI Analyta Analyta Analyta - Analyt 5.310 20 - a . -*B90 --------18 20.260 17.684 mx MMX Analyta Analyta Analyt 5.291 5.275 5.254 20 20.376 47 47.425 47 47.000 MMX MMX MMI QC 49.30 Analyt Analyt 5.256 $.287 17 17.200 17 16.612 MMX MMX QC 49.30 Analyt Analyta Analyt Standard 4.93 Standard 9.76 Standard 24.80 Standard 49.30 Standard 97.60 Png 2 frk s t i l l i ! oup 0J0159: :quntittd and printad by mjm 004341 Quantify Compound Suanary Raport Rat U n n o Mathod Davalopnant, SSS Saapla Lit: S:\PACT-l.PR0\SaMplaOB\OSO399b Laat modifiad: Mon May 03 10:01:10 1090 Mathod: S:\PACT-l.PRO\MathOB\050399b Laat nodxflad: Tua May 04 11:00:31 1990 Job Coda: Pnntad: Pri May 21 11:54:44 1999 Compound 3: MS 13 1 Naaa flaiaplallat Tazt 1 050390006 MaOH Blank 2 OS0399007 MaOH Blank 3 050399008 GEN011 RBS04289-MBlank-i 4 050399009 GEN011 RBS04289-SBlank-l S 050399010 G E N O U RBS04289-5 ppb-1 6 050399011 G E N O U RBS04289-10 ppb-1 7 050399012 G E N O U RBS04289-25 ppb-1 8 050399013 G E N O U ABS04289-50 ppb-1 9 050399014 G E N O U R8S04289-100 ppb-1 10 050399015 MaOH Blank 11 050399016 MaOH Blank 12 050399017 G E N O U ABS04289-WBlank-l 13 050399018 GENOU, 9394 (0.09 aL) 14 050399019 GENOU, 9395 (0.07 aL) 15 050399020 GENOU# 9396 (0.08 aL) 16 050399021 GENOU# 9397 (0.07 aL) 17 050399022 GENOU# 9398 (0.07 aL) 18 050399023 G E N O U RBS04289-50 ppb-1 19 050399024 MaOH Blank 20 050399025 G E N O U RB304289-NBlank-l 21 050399026 GENOU# 9399 (0.07 aL) 22 050399027 GENOU, 9400 (0.07 aL) *3<O8W9900-~1 *~- GENOU, 9401 (0.08 aL) ... 24 050399029 GENOU# 9402 (0.08 aL) 25 050399030 GENOU# 9403 (0.07 aL) 26 050399031 G E N O U RBS04289-50 ppb-1 27 050399032 G E N O U RBS04289-250 ppb# MB 28 050399033 G E N O U RBS04289-250 ppb# MSO 29 050399034 G E N O U RBS04289-50 ppb-1 30 050399035 MaOH Blank 31 050399036 G E N O U RB504289-NBlank-2 32 050399037 G E N O U RB504289-S81ank-2 33 050399038 G E N O U RB504289-5 ppb-2 34 050399039 G E N O U RBS04289-10 ppb-2 35 050399040 G E N O U RBS04289-2S ppb-2 36 050399041 G E N O U RBS04289-SO ppb-2 37 050399042 G E N O U RBS04289-100 ppb-2 BESTCOPYAVAILABLE - ._ Typa Analyta Analytt Analyta Analyta Standard Standard Standard Standard Standard Analyta Analyta Analyta Analyta Analyta Analyta Analyta Analyta QC Analyta Analyta Analyta Analyta Analyta Analyta Analyta QC Analyta Analyta QC Analyta Analyta Analyta Standard Standard Standard Standard Standard Std Cono 4.93 9.76 24.80 49.30 97.60 49.30 49.30 49.30 4.93 9.76 24.80 49.30 97.60 Axaa Raaponaa Paga 3 Plaga %Dav * S/Ul-fi aoup 020190;jq u a n tita ta d and p rin tad by h . 0 W 0 004342 Q u a n tify Compound l u m t r y R a p o r t Rat U rin a H athod D a v e lo p a ie n t, SEE Saapla U a t : a:\rACT-l.mo\fMplaOB\0S039Sb Last odlflad: Mon May 03 16-.01:10 199 Mathod: :\rXCT-l. K A M . ChO0\OSO39b Last modi find: Tu May 04 11:00:31 1999 Job Coda: Printed: Pri May 21 11:54:44 1999 Compound 4 : aurr 1 Maiaa 1 050399004 2 050399007 3 050399008 A 050399009 5 050399010 6 050399011 7 050399012 8 050399013 9 050399014 10 050399015 11 050399014 12 050399017 13 050399018 14 050399019 IS 050399020 14 050399021 17 050399022 18 050399023 19 030399024 20 050399025 21 050399026 22 050399027 24 050399029 25 050399030 26 050399031 27 050399032 28 050399033 29 050399034 30 050399035 31 050399036 32 050399037 33 050399038 34 050399039 35 050399040 36 050399041 37 050399042 . aaplaliat Tact MaOH Blank HaOH Blank G E N O U R8S04289-WBlank-l G E N O U RBS04289-SBlank-l G E N O U RBS04289-S ppb-1 GEN011 RBS04289-10 ppb-1 GEN011 RBS04289-2S ppb-1 G E N O U RB504289-50 ppb-1 G E N O U RBS04289-100 ppb-1 MaOH Blank MaOH Blank G E N O U RBS04289-tfBlank-l G E N O U , 9394 (0.09 r L) GENOU, 9395 (0.07 *L) GENOU, 9396 (0.08 RL) GENOU, 9397 (0.07 r L) GENOU, 9399 (0.07 r L) G E N O U RB504289-50 ppb-1 MaOH Blank G E N O U RBS04299-NBlank-l GENOU, 9399 (0.07 mL) G E N O U , 9400 (0.07 r L) G E N O U , 9401 (0.09 r L) G ENOU, 9402 (0.09 r L) GENOU, 9403 (0.07 *L) G E N O U RBS04289-S0 ppb-1 G E N O U RBS04289-250 ppb, M5 G E N O U RBS04289-250 ppb, MSO G E N O U RB504299-50 ppb-1 MaOH Blank G E N O U RB504289-NBlank-2 G E N O U RBS04289-S81ank-2 G E N O U BBS04289-S ppb-2 G E N O U RBS04289-10 ppb-2 G E N O U RBS04289-25 ppb-2 G E N O U RBS04289-50 ppb-2 G E N O U RBS04289-100 ppb-2 SEST COPY AVAILABLE - 4 Typa Analyta Analyta Analyta Analyta Standard Standard Standard Standard Standard Analyta Analyta Analyc*Analyta Analyta Analyta Analyta Analyta OC Analyta Analyta Analyta Analyta Analyta Analyta Analyta oc Analyta Analyta QC Analyta Analyta Analyta Standard Standard Standard Standard Standard Btd Cone RT 1.00 1.00 1.00 1.00 1.00 5.016 5.008 5.022 5.002 5.009 5.005 5.022 1.00 5.010 5.012 5.004 5.012 5.012 5.012 5.006 5.032 5.007 -- - -:-s?r5is 4.998 5.006 1.00 5.016 5.010 5.013 1.00 5.007 1.00 1.00 1.00 1.00 1.00 5.026 5.008 5.014 5.023 5.006 5.027 5.013 Araa Raaponaa 1624 1839 1769 1875 1791 1535 1891 1624.026 1839.452 1769.446 1875.130 1790.798 1535.177 1890.829 1893 3937 4584 4072 4269 3633 1782 217 425 __A9JU 5032 4395 7774 1979 4326 3993 2442 1996 2227 2203 2162 2241 2449 2194 1993.356 3937.170 4583.925 4072.485 4269.604 3633.260 1781.550 -a*. 2179.890 4257.904 4943.963 5032.093 4394.549 7774.321 1979.790 4326.159 3993.073 2442.139 1996.270 2226.930 2202.940 2161.525 2241.125 2446.654 2194.037 Cono. Plaga IDav 0.81 bb 0.91 bb 0.98 bb 0.93 bb 0.69 bb 0.76 bb 0.94 bb -19 -9 -12 -7 -U -24 -6 0.94 bb 1.96 bb 2.29 bb 2.03 bb 2.12 bb 1.81 bb 0.89 bb 1.08 bb 2.12 bb 2.41 bb 2.50 bb 2.19 bb 3.87 bb 0.96 bb 2.15 bb 1.99 bb 1.21 bb 0.94 bb 1.11 bb 1.10 bb 1.07 bb 1.11 bb 1.22 bb 1.09 bb -6 96 128 103 112 91 -U 8 112 141 ISO 119 287 -2 115 99 21 -6 U 10 7 11 22 9 k,h 5 /U ,'V aoup 020199: :quan ti ta tad and p r in ta d by m i 004343 9 Vh tON r4 fk S joojo n S a u xi u ii S 32SSS3 SSS3 m o r* r* M A A N A WO r*f*HHO 0 HVN A A mo*o 4 O N N h H lfl V A AA V 1. 1. 1. S VOWOA HN A A o O ONAOs h h V A A NA A NOM m mo* Nhr"* * r ffnor h & V I" W W (D ifl rth H* MNlOO 2 iAiahr n <ah h h i Ah o n o *OMf-**n NN NOINACD wocnw HNnot iftMhH HhNAH HdiAHONn WM|Htf) NN Nftn AA IDOMAtt Hnia A I A ( A tf> t ft lO ) i >m intfir-mv'rr <V9 wvww w w tOMliAlAiAlAlA <oo ma m 9A9h V WV w <o mia u) V)ia TJTJTJTJTJ OOOMMbl4W0OOOOOO MWiiwywwP4>y > >i ><>TJTJTJTJT) ><>i >i >i >i >>i >i -4 -4 ,H -H C C C C -- + +m > I 4 4J *J >% > TJTJTJTJTJ OMMbMM V .t it m m m m >*>*>.V TJV V TJ ; Ig C6 >V) CffV) S j SS *4r4 H rl H I MM N MMN I I I * I I I J1 m m i a o a cl M M 7 JQJ>il *8. c e Aa aa aa aa a -ChD-0*3a o OAOO SAA rl NApl 2232S8: 5--d-d--d - s M OO SS-SSft H H ft O 8 8rO- Or- O OOAo NoNmAo Ma rtHo NoAeHo 919t O* o*o o o o o c w w p w w QD I .....................I I I I OAAO OW OW OWOWAGAG#AG9GAB t it illi AAAAAAA a NNNNNN MM MMMM M M M MM M M A r*a T AOHNATTf T MM OOOOOOO AAAAAO OOtOOOOOOOO I (AA ) V) I ) J( J<0)n n n n n n jtn n a tA v n w H n .. ___________ .. S C ->m S S S S S S S S SS cggggggg HHH ItfA H rlrlP lH H H * *4 m 4 -4 .4 ............................ .* HHHHHHflHHHHHHHHHHflHHHHHHH rt HHHHp-4 HHHr*4ri p*p4p-4Hp4 p4HHHHHH ZOOOOOOOXS o o o o o o s o o o o o o o o o o x o o o o o o o 1 '2325352'^ 2 5 2 3 2 3 J 2 S 3 2 2 2 2 2 2 S 2 2 2 2 2 2 2 Z I J O O J u o 6 o o o z t f S i S 5 o o t J O o 5 x i 3 u o i 3 U u o n v A W r a A O H N n v or* A OHNp>*r w>mAA* m*o*0*0*0*0 >ooo o o o o o c A O*o*o*cr*o*O* O* G ooOOCo o 0 O O G o*o*O* O* G A 9*9* 01 01G *0*O*0*9*O*0*O O* G o*o*0*01<O*01010101 < o<nn r ri r* ri n f r>n r>n f n n n n n f >ooo o o o o o oooo oo o o ooo < >*o*> OlO >o o oo iO o *oo oo oo nooAA* ooooo O C iOiOAAAl o o OOOG r> o*o hm r* * n *o r* D o* *0*0*0o r* r r r - r* r-r* r r f- oooo o o o o ooo o o o 0*0*0*010*0*0*0* o* o* 010*0*0* 0*0*0*A O*O*A A o* o* A A A A r* r*r* n rta rt M n ri A A A A oA Ao oo AoOOAo AOo AoOAoOAoOaoo o m o o oOO AAAA oo oO N n t A M D O I O p i N n A h e <i^1 vy r 4M1*1* n oo a in nT ' eup 020199: :qu*nti.t*t*d and printed by w i|flV