Document gLbd8M1d9G1EDgBMz7gx3YyG

- 0664- FOSA or PFOSA Ongoing - / 000502 3M MEDICAL DEPARTMENT, CORPORATE TOXICOLOGY Protocol for Study No. T-7132.2; ST-39 PHARMACOKINETIC STUDY OF PERFLUOROOCTANE SULFONAMIDE IN RATS Study Objective: The objective o f this study is to assess the potential for oral absorption, urinary and fecal clearance and biological persistence o f Perfluorooctane Sulfonamide (PFOSA) in male Sprague Dawley rats after a single oral dose. Analysis o f the serum, liver, urine and feces for potential metabolites o f PFOSA will be performed by LCMS and perhaps other methods. Previous studies o f the N-ethyl derivative o f PFOSA have concluded that PFOSA is the ultimate metabolite in rats (1,2); however, the analytical technique used in these studies was unable to detect all potential metabolites, including perfluorooctanesulfonate (PFOS). N o pharmacokinetic studies have yet been done on PFOSA to resolve this issue and search for other possible metabolites in the urine and feces. Recently, validated methods have been developed for the quantitation o f PFOSA and its potential metabolite, PFOS, in serum and liver down to the low part per billion level (3). One goal o f this study is to determine the potential for, if occurring, the extent o f conversion o f PFOSA to PFOS. This information will help to explain the pharmacokinetics o f NEtFOSE and its metabolites and provide data for proper risk characterization. Research Client: 3M Specialty Chemicals Division 3M Center, Building 236 Saint Paul, MN 55144 Sponsor: Study Location: 3M Specialty Chemicals Division 3M Center, Building 236 Saint Paul, MN 55344 3M Strategic Toxicology Laboratory 3M Center, Building 270-3 S-06 room SB314 Saint Paul, MN 55144 Study Director: Andrew M. Seacat, Ph.D. Toxicology Specialist 3M Medical Dept. / Corporate Toxicology 3M Center, Building 220-2E-02 Saint Paul, MN 55144 Ph.: 651-575-3161 FAX: 651-733-1773 Study Toxicologist: Deanna Luebker, MS Advanced Research Toxicologist 3M Medical Dept. / Corporate Toxicology 3M Center, Building 220-2E-02 Saint Paul, MN 55144 000503 Ph: 651-737-1374 FAX: 651-733-1773 T-7132.2; ST-39 PFOSAPK Proposed Study Timeline In-Life Start Date: October 4th, 1999 In-Life End Date: November 2nd, 1999 Analytical Completion Date: TBA Final Report Completion Date: TBA Regulatory Compliance: This study will be performed in the 3M Strategic Toxicology Laboratory under a defined protocol and classified as a "Class B Study" as explained in TOX SOP 0950, Strategic Toxicology Lab GLP Program Procedure. Test M ateriali Dan Hakes. Product Responsibility Liaison 3 M Chemicals Division, w ill furnish high-purity PFOSA. Identification: Name: Perfluorooctanesulfonamide Molecular Formula: CsF17S02NH2 Lot Number: L -10009 (Prepared by George Moore, 3M SMD Lab, Bldg 236, April 1996) Purity: Analysis by GCMS determined that the staring material was over 99% pure (4). Qualitative and quantitative compositional results that were derived from the single trial *H/19F-NMR cross-integration analysis revealed that the composition was 65.8% CF3(CF2)x-S02-NH2 (Normal chain), 18.7% CF3(CF2)x-CF(CF3)-(CF2)y-S02-NH2 (Internal monomethyl branch), 11.2% (CF3)2CF-(CF2)x-S02-NH2 (Isopropyl branch), 3.5% CxF2x+l-CF(CF3)-S02-NH2 (Alpha branch) and 0.28% (CF3)3C-(CF2)x-S02-NH2 (t-Butyl branch)(5). HPLC/MS characterization o f the PFOSA sample revealed 9,600 ppm o f PFOS, 1,100 ppm o f C7F15SO2NH2, 510 ppm o f C9F19SO2NH2, 6,600 ppm o f CgFi6HS02NH2, 24,000 ppm o f C18F36HSO2NH2, 1,200 ppm o f CgFi5H2S02NH2 and lower concentrations o f several other amides. Based on the sum o f the impurities, the purity o f the PFOSA sample would be approximately 96 % (6 & appendix I). Stability: Documentation will be kept on file with the Sponsor. Storage Conditions: Upon receipt, test material will be stored tightly sealed at room temperature. Characteristics: Information on synthesis methods, composition or other characteristics that define the test material will be kept on file with the Sponsor. 2 00050^ A n im als: Species: Rat Strain: Sprague Dawley Source: Harlan Age at initiation of treatment: Weight at initiation of treatment: Number and sex: 30 males 6-8 weeks approximately 150-250g T-7132.2; ST-39 PFOSA PK Table 1 - Dose Groups Group Dose 1 0 mg/kg 2 5 mg/kg N 15 15 Euthanasia 5 each on days 1, 4 and 29 post dose 5 each on days 1, 4 and 29 post dose Identification: AUA Number: ear tag with animal number or unique tail mark. 2246 Husbandry: Housing: All rats from groups 1 and 2, which are to be sacrificed on day 29 post dose, will be housed individually in metabolism cages for portions o f the study (see Table 2). When not in metabolism cages, these rats will be group housed in standard cages. All other rats will be group housed in standard cages throughout the study. Diet/Water: Harlan Teklad LM-485 Mouse/Rat Sterilizable Diet, supplied by Harlan Teklad, Madison, WI, and tap water will be provided to all rats a d libitum throughout the study. Environment: Environmental controls for the animal room will be set to maintain a temperature o f 72 3F, humidity o f 30-70%, a minimum o f 10 exchanges o f room air per hour and a 12 hour light/dark cycle. Dose and Dosing Procedures: Method of administration/Dose preparation: A single 5mg/kg dose o f PFOSA will be administered via oral gavage to rats in group 2 on day zero o f the study. The PFOSA will be prepared from a stock solution o f 1^Omg/ml PFOSA in acetone A final 0.1 % (InWmH uniform suspension (or emulsion) o f PFOSA in 2% Tween 80 and 1% acetone will be prepared using a 15 ml dounce tissue grinder. A volume o f 5 ml suspension / kg body weight will be administered to each rat. Re suspension o f solids will be performed with 5 strokes o f the tissue grinder pestel before each sample is drawn-up in the syringe for dosing. A single 5 F 00505 T-7132.2; ST-39 PFOSAPK ml / kg body weight dose o f vehicle, 2% Tween 80 and 1% acetone, will be administered via oral gavage to rats in group 1 on day zero o f the study. Observation o f Animals: Clinical Observations: Each animal will be observed daily (excluding weekends and holidays) for mortality and morbidity and notable findings will be recorded. Additional findings will be recorded as they are observed. Body Weights: Each animal will be weighed immediately prior to treatment, weekly thereafter and immediately prior to euthanasia. Specimen Collection: Frequency (See table 2): Urine and feces collections will be made on days 1 - 4 post dose Necropsies will be performed on days 1, 4 and 29 post dose. Table 2 - Schedule Sun Oct 3 Mon Oct 4 day 0 DOSING Oct 10 dav 6 PD Oct 17 day 13 PD Oct 11 day 7 PD Oct 18 day 14 PD Tues Oct 5 day 1 PD Collection, Dy 1 PD sac Oct 12 day 8 PD Oct 19 day 15 PD Wed Oct 6 day 2 PD Collection Oct 13 day 9 PD Oct 20 day 16 PD Thurs Oct 7 day 3 PD Collection Oct 14 day 10 PD Oct 21 day 17 PD Fri Oct 8 day 4 PD Collection Switch to reg cages. Dy4PD sac. Oct 15 day 11 PD Oct 22 day 18 PD Sat Oct 9 day 5 PD Oct 16 day 12 PD Oct 23 day 19 PD Oct 24 day 20 PD Oct 31 day 27 PD Oct 25 day 21 PD Nov 1 day 28 PD Oct 26 day 22 PD Nov 2 day 29 PD Dy 29 PD sac. Oct 27 dav 23 PD Oct 28 dav 24 PD Oct 29 day 25 PD Oct 30 day 26 PD Method of Specimen Collection: Urine and feces will be collected from each metabolism cage at the designated times. The initial volume o f urine will be recorded, the sides o f the urine collection apparatus will be washed with approximately 5- 10ml deionized water and the final volume of urine vvi!! be brought to 15 ml with additional deionized water. Daily feces weight will be recorded for each animal. At the designated times, animals will be euthanized by CO2 and gross necropsy performed. During necropsy, blood ( 6 ml) will be collected via the abdominal aorta and transferred to blood collection tubes without anticoagulant. Blood samples will be allowed to clot for a period 4 OOO506 T-7132.2: ST-39 PFOSAPK of 15 to 30 minutes at room temperature and the dot will be spun down in a centrifuge at 1100 x g for 5 minutes. The serum will be transferred to labeled 1.5 ml microfuge tubes and centrifuged again at 2000 x g to remove any remaining red blood cells. Each sera sample will then be transferred to a separate labeled polypropylene microfuge tube and frozen in dry ice. Livers will be removed, weighed, placed individually into labeled sterile sample bags and flash frozen in liquid nitrogen then maintained on dry ice. Specimen Handling: Specimens will temporarily be stored in a freezer set to maintain -60 to 80C. For metabolite analysis, these specimens will be packed in dry ice and shipped to. Kris Hansen, Ph D 3M Environmental Technology and Safety Services 935 Bush Avenue St. Paul, MN 55133-3331 Ph: 612-778-6081, FAX: 612-778-6176. All results will be provided for inclusion in the final report. The number, type and date o f collection o f specimens to be generated for analysis are as follows. Table 3 - Specimens Specimen day 1 post dose Serum 10 (5/group/day) Liver 10 (5/group/day) Urine 10 (5/group/day) Feces 10 (5/group/day) day 2 post dose 10 10 Day 3 post dose 10 10 day 4 post dose 10 10 10 10 day 29 post dose 10 Total 30 10 30 40 40 Data Analysis: Data collected on parent compound and identifiable metabolites will be analyzed fr*r toxicokinetic parameters and for statistically significant differences between groups using ANOVA and /or Students T-test. 5 000501 T-7132.2; ST-39 PFOSA PK Responsibilities: Deanna Luebker and Andrew Seacat will be responsible for dosing the animals, collecting in-life specimens, performing the necropsies and collecting and sending tissue specimens for analysis. Kris Hansen, 3M Environmental, will be responsible for analytical evaluation o f the Andrew Seacat will draft a final report and ensure the report receives appropriate 3M review before a final report is issued. U00508 6 * Signatures: T-7132.2; ST-39 PFOSA PK O f). Andrew M. Seacat Ph D. Toxicology Specialist Study Director -j- / ?* ? Date ______________ f p / & 7 Deanna Luebker, MS Advanced Research Toxicologist Study Toxicologist Date 000509 7 * T-7132.2; ST-39 PFOSA PK References: 1. Grossman M.R. and Bowen J.M. (1990) Tissue analysis o f fluorinated sulfonamide pesticide: an evaluation o f distribution, elimination, and potential for bioaccumulation in orally exposed rats. M.S. Thesis, Univ. o f Georgia, Athens, GA. (also possibly published as: Grossman Mark R. and Bowen J.M. (1990) Tissue distribution and elimination o f a fluorinated sulfonamide pesticide in rats. Fundctm. Appl. Toxicol., but notfound). 2. Grossman M.R., Mispagel, M.E. and Bowen J.M. (1992) Distribution and tissue in rats during and after prolonged dietary exposure to a highly fluorinated sulfonamide pesticide. J. Agric. Food Chem. 40, 2505 - 2509. 3. K.J. Hansen, L A. Clemen, M E. Ellefson, H O. Johnson. (1999). Compound Specific Characterization o f Organic Fluorochemicals in General Population Human Sera Samples. 3M Environmental Lab, St. Paul, MN 55133. 4. Payfer R.M. GC/MS analyses o f PFOSA (L -10009). SA&C Analytical Request No. 59426. Report 9/24/99. 3M SA&C Lab Building 236-2B-11. 5. Tom Kestner Chemical Characterization o f PFOSA, L-10009, by 1H and 19FNMR Spectroscopy Requests # 59426. 3M Specialty Adhesives & Chemicals Analytical Laboratory / SMMD-236-2B-11, September 25, 1999. 6. DeRoos F.L. Characterization o f PFOSA Samples, T-7132-1 (L-10009) and TNA-1584. Request # A-151254. Report 10/7/99. Corporate Analytical Technology Center, Building 201-1-29, CATC - Chromatography Group. 8 000510 Appendix I: Tel: 736-0665 201-1W -29 T-7132.2; ST-39 PFOSA PK Corporate Analytical Technology Center To: Larry A. Wendling/US-Corporate/3M/US cc: Andrew Seacat/US-Corporate/3M/US Subject: Characterization of PFOSA Sample for Toxicology Larry, I have completed the HPLC/MS characterization of the PFOSA sample (T-7132-, L-10009 prepared by G. Moore 4/96) that is proposed to be used for the animial feeding study. I found 9,600 ppm o f PFOS, 1,100 ppm o f C7F^5S0 2NH2, 610 ppm o f C9F ig S 0 2 NH2> 6,600 ppm of CgF'|gHS0 2 NH2, 24,000 ppm of C-tgF3gHS0 2 NH2 , 1,200 ppm o f c 8f 15^2s o 2n h 2 and lower concentrations of several other amides. Based on the sum of the impurities, the purity of the PFOSA sample would be approxim ately 96 %. I've thought a little more about apparent presence of C 18F36H SO 2NH2 in the sample. The identification of this compound was based primarily on the observed molecular weight and the relative elution order in the chromatogram. Rather than C 18F36H SO 2 NH2 , it seems more probable that this compound is actually (C sF 17S 0 2)2N H - Confirmation of this identification will require additional analyses. I also need to think more about whether the other partially hydrogenated perfluoroamides may actually be of this The PFO S was quantified using a standard curve prepared by analyzing P F O S standards so its concentration should be accurate. The amide impurities, however, including the partially hydrogenated amides, were all quantified using a PFOSA standard curve assuming that they had the same mass spectral response factor as did PFOSA. W hile this assumption will introduce some error to the quantitative data, it is the best we can do since we do not have standards for each of these amides. Also, this calculated purity assumes that all of the impurities are amenable to HPLC and are detected by the analysis. W hile not always true, this sample was analyzed by Rick Payfer using G C /M S and by CATC using our GC method. Neither of the analyses found volatile or semivolatile impurities, e.g., N-methyl FO SE, Nethyl FOSE, etc. at concentrations greater than 50 ppm. I also carried out a semiquantitative assessment of the purity of the PFO S A by comparing the PFOSA response to a PFOSA standard curve. Using this technique, the purity of the PFOSA sample was found to be 118 %. These analyses were carried out in duplicate, with triplicate injections of each solution, so they should be relatively accurate as analytical variation would be averaged. In general, however, it is not highly accurate to use a chromatographic method to quantify a relatively pure material due to the extremely large dilution factor, in this case >100,000, that must be applied. It is not expected that instrumental variation would bias the purity high. It is possible that the purity of the sample is actually higher than the purity of the PFO SA that we are using as a standard! If this were true, the purity would be determined to be > 100%. Andrew Seacat has reviewed the concentrations of the impurities that were determined and calculated that the concentration of PFO S will not adversely affect the study. At 9,600 ppm, he calculates that the rats receiving 3 mg/kg/day would ingest app. 0.20 mg P FO S total in 9 O O O S l^ J  T-7132.2; ST-39 PFOSA PK Appendix I Continued: 28 days assuming a 0.25 kg rat. If we further assume that 30 % of that is deposited in the liver (based on previous feeding studies) and liver is approximately 12 grams, then the predicted concentration in the liver from the residual PFOS would be 200 ug PFO S x 0.3 / 1 2 g liver weight = 5 ug/gram, or 5 ppm, which in itself should not impose any toxicological consequences. Any PFOS measured significantly over that could be attributed to metabolism of PFOSA to PFOS. He believes that the 1-H and 2-H perfluoro amides are interesting as they may be subject to metabolic attack, however these amides should be analytically distinct from the Perfluorinated species on down the line, and would not amount to a foreseeable toxic concentration and therefore would be acceptable if no other substitute can be prepared. Andrew is still thinking about whether the (CgF-)7S02)2N H will have a negative impact on the study. Please give me a call at 6-0865 it you have any questions concerning our analyses or if i can provide additional information. Fred L. DeRoos CATC 10 **0512. Laboratory Report Analytical Report of Data for PFOSA Pharmacokinetic Study in Rats (Sera and Liver) Laboratory Report No. FACT-TOX-145 (W2814) Requester Project No. T-7132.2 Testing Laboratory 3M Environmental Technology & Safety Services 3M Environmental Laboratory Fluorine Analytical Chemistry Team (FACT) 2-3E-09 935 Bush Avenue, St. Paul, MN 55106 Laboratory Contact Kris Hansen, Ph.D. Bldg. 2-3E-09 P.O. Box 3331 St. Paul, MN 55133-3331 Phone: (651)778-6018 FAX: (651)778-6176 R eq u ester Andrew Seacat and Deanna Luebker 3M Company Toxicology Services 220-2E-02 St. Paul, MN l OF6 000513 1 Introduction This study was designed to preliminarily assess the adsorption and metabolism by the Sprague Dawley rat of the perfluorooctanesulfonyl amide (PFOSA, Q F 17SO2NH2, CAS # 31506-32-8). Test animals were dosed by oral gavage with 5 mg/kg of PFOSA suspended in 2% TWEEN 80; control animals were given 2% TWEEN 80 with no PFOSA. Subsets of the dosed group and the control group were sacrificed on day 1, day 4, and day 29 post-dose. Sera and liver collected from the sacrificed animals were sent to the Environmental Lab and analyzed quantitatively for perfluorooctane sulfonate (PFOS, CgFnSQf, CAS # 2795-39-3), PFOSA, and perfluorooctanoate (POAA, C7Fi5C0 2\ CAS # 2991-51-7). PFOS and PFOSA were detected in the livers of all dosed animals. PFOS levels were highest in the day 4 group, but even liver from animals sacrificed 29 days post dose were determined to contain high levels of PFOS. PFOSA levels in the livers of the dosed animals were highest in the group sacrificed on day 1; on day 29, the average PFOSA level was approximately 2.5 % of the day 1 levels. POAA was not detected above the lim it of quantitation in the livers of dosed animals. As in the liver extracts, sera extracts collected 4 days post-dose evidenced the highest PFOS levels. Serum PFOSA levels decreased from day 1 to day 4 to day 29; on day 29, sera from four out of five animals did not contain PFOSA above the lim it of detection. POAA was detected in the sera of animals collected on day 1 and day 4. Screening studies of the dose material suggest that a small amount o f POAA was present in the PFOSA dosing solution PFOSAB, (QFnSOxfeNH, was detected in the livers of dosed animals. This analyte was also present in the solution used to dose the animals. No investigations of PFOSAB in the sera were conducted. The solution used to dose the test animals was analyzed to confirm the theoretical dose levels. The PFOSA concentration in the TWEEN 80 solution was determined to be 1330 +/- 400 pg/mL. PFOS and POAA were also identified in the dose solution. The concentration of PFOS was estimated to be approximately 18.5 pg/mL; POAA levels are approximated at 2.5 pg/mL. PFOS and POAA data were collected from a single analysis and should be considered to be o f screening quality only. A more thorough characterization of the material used to dose the animals was requested by 3M Toxicology and was conducted by Fred Deroos prior to initiation of the study. Results of this more comprehensive characterization are available from the requestors. Although rigorous quality control measures and 3M Environmental Laboratory Standard Operating Procedures were followed, the acquisition of this data was not necessarily collected according to applicable Good Laboratory Practices. Neither the dose material nor the analytical standards were given a certificate of analysis; dose material was characterized by NMR and LCMS and the analytical standards were characterized by NM R The data presented here is not suitable for distribution to any government agency in defense of product suitability or safety. This data is the highest quality data available at this time. 2 Sam ple Receipt On 10/6/99,10/8/99, and 11/1/99 Deanna Luebker from 3M Toxicology Services shipped rat urine, feces, liver, and sera, samples to the FACT group in the 3M Environmental Laboratory; samples were received frozen on dry ice and were stored at -20 C. 3 Holding Tunes There is no holding time criteria associated with these samples for LC/ESMSMS analysis. 2 OF6 000S14 M ethods - A nalytical and Preparatory Analytical methods ETS-8-4.1, Extraction of Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds from Serum for Analysis Using HPLC-Electrospray/Mass Spectrometry ETS-8-6.0, Extraction of Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds from Liver for Analysis Using HPLC-Electrospray/Mass Spectrometry ETS-8-5.1, Analysis o f Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Serum Extracts Using HPLC-Electrospray/Mass Spectrometry ETS-8-7.0, Analysis o f Potassium Perfluorooctanesulfonate or Other Fluorochemical on Liver Extracts Using HPLC-Electrospray/Mass Spectrometry Sample preparation -HPLC/ESMSMS: ion-pairing extraction Analyte is extracted from sample matrix with ion pairing reagent [tetrabutyl ammonium hydrogen sulfate (TBA)] in a pH-controlled environment The cationic reagent selectively targets anionic fluorochemicals. Once the anion-TBA pair is formed, the analyte is transferred into a non-polar organic solvent (methyl-ierfbutyl ether), dried, and reconstituted in methanol for MS analysis. HPLC/ESMSMS In HPLC, an aliquot of extract is injected and passed through a reverse phase liquid chromatographic column. Based on the affinity o f the analyte for the stationary phase in the column relative to the liquid mobile phase, the analyte is retained for a characteristic amount of time. For example, in a standard solution PFOS may elute at 8.0 minutes. Retention times between a standard PFOS solution and the analyte extracted from tissue 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 of 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 (Q F 17SO3) analysis, ion 499 is selected as the characteristic primary ion. This ion is fragmented into other ions such as 80 amu (corresponding to SO3'), and 230 amu (CjF6S03> Each of these secondary fragments is detected and can be used to differentiate PFOS from other compounds that might have the same characteristic 499 amu primary ion, but different chemical compositions and secondary ion fragmentation patterns. 4 Analysis 4.1 Calibration 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 in the response of one or more specific daughter ions using the multiple response-monitoring mode of the instrument A mid-level, extracted matrix calibration check standard is analyzed every 5-10 samples to monitor instrumental drift. Calibration check standards are compliant if instrumental response is within +/- 30% of the expected value. 3 OF6 000515 4.2 Blanks Two extraction blanks, utilizing water as surrogate matrix, are extracted w ith each batch o f samples. Additionally, two samples of blank matrix (both liver and sera) are extracted along with each batch o f samples and curves. Blanks are compliant if no target analyte is detected above the lim it o f detection for a specific analyte. In this study, all blanks were compliant. 4.3 Surrogates Tetra-hydroperfiuorooctanesulfonate is used as a surrogate in this analysis. Surrogate response is monitored to confirm gross instrumental M u re, if necessary. In the non-diluted samples, the surrogate response was acceptable (+/-50%) for all analyses. 4.4 Matrix Spikes Duplicate matrix spike analyses utilizing all target analytes were prepared and analyzed for one control animal. W ith one exception, PFOS recoveries were within the acceptable range of 70-130%. One liver matrix spike showed a 66 % recovery for PFOS. All PFOSA matrix spike recoveries were acceptable for PFOSA. As POAA was not a target analyte in this analysis, no matrix spikes were prepared Although the recovery of POAA from sera and fiver has been verified for other studies, POAA results should be considered screening quality only. One matrix spike was prepared for each of the target analytes in the dose verification study. Spike recovery for PFOSA was 130%, PFOS was 115%, and POAA was 121%. 4.5 Laboratory Control Samples Laboratory Control Samples are not a component of this study. 4.6 Sample Related Comments Other matrices submitted with this study will be analyzed as needed upon written request from the sponsors. In the event of further analysis, an additional report will be generated Dose verification was conducted by evaluating diluted aliquots of the dose against an unextracted standard curve. Triplicate dilutions of the TWEEN 80 dose solution were analyzed for determination o f PFOSA; a single dilution was analyzed for determination of PFOS and POAA S D ata Summary The table of results detailing the sera analysis is available in Attachment A. Results of the liver analysis are presented in Attachment B. PFOS and PFOSA were detected in the livers of all dosed animals. PFOS levels were highest in the day 4 group, but even day 29 group animals were determined to contain high levels o f PFOS. PFOSA levels in the livers of the dosed animals were highest in the group sacrificed on day 1; on day 29, the average PFOSA level was approximately 2.5 % of the day 1 levels. POAA was not detected above the lim it of quantitation in dosed animals. As in the fiver extracts, sera extracts collected 4 days post-dose evidenced the highest PFOS levels. Serum PFOSA levels decreased from day 1 to day 4 to day 29; on day 29, sera from four out o f five animals did not contain PFOSA above the lim it o f detection. POAA was detected in the sera of animals collected on day 1 and day 4. Screening studies o f the dose material suggest that a small amount of POAA was present in the PFOSA dosing solution PFOSAB was detected in the livers o f dosed animals. This analyte was also present in the solution used to dose the animals. No investigations o f PFOSAB in the sera were conducted. 4 OF6 000516 The solution used to dose the test animals was analyzed to confirm dose levels. The PFOSA concentration in the TWEEN 80 solution was determined to be 1330 +/- 400 pg/mL. PFOS and POAA were also identified in the dose solution. The concentration o f PFOS was estimated to be approximately 18.5 pg/mL; POAA levels are approximated at 2.5 pg/mL. PFOS and POAA data were collected from a single analysis and should be considered to be of screening quality only. 6 Data Qualify Objectives and Data Integrity No circumstances existed during the present study that would have adversely affected the quality or integrity o f the data. The following data quality objectives were followed during the study: Linearity - The correlation coefficient (i*2) of the standard curve was equal to or greater than 0.98 using 1/x weighting Limits of detection (defined as Vi the LOQ) - PFOS in sera is 4.88 ng / mL; PFOS in liver is 15.3 ng / g; PFOSA in sera is 2.47 ng / mL; PFOSA in liver is 6.2 ng / g Limits of quantitation (defined as the lowest extracted standard accurate to within 30% o f theoretical value) - PFOS in sera is 9.76 ng / mL; PFOS in liver is 30.7 ng / g, PFOSA in sera is 4.93 ng / mL; PFOSA in liver is 12.4 ng / g Duplication fiequency/acceptable precision - < 30% Spike fiequency/acceptable recoveries - 70% to 130%; PFOS recoveiy was 66 % for a single matrix spike in liver (see Section 4.4) Use o f confirmatory methods - no confirmatory methods were used Demonstration of specificity - specificity was demonstrated by chromatographic retention tim e and mass spectral characterization of a single product ion Given the parameters listed above, and assuming spike recoveries form a suitable indication o f endogenous analyte recovery, data are quantitative to +/- 30%. The validity of this assumption has not been verified by other techniques. 7 Attachments Attachm ent A: Table of results o f sera analysis Attachm ent B: Table of results of liver analysis A ttachm ent C: Sample receipt A ttachm ent D: Screening results of dose verification A ttachm ent E: Extraction and analytical data 5 OF6 000517 8 Signatures C tfiia A Clur>*A~._____________________________ _________ la / o J f o ______________ Lisa Clemen, Advanced Chemist D ate / < - H z . ------------- Kris Hansen, Ph D., Principal Analytical Investigator D ate 6 OF 6 000518 Laboratory Report Analytical Report of Data for PFOSA Pharmacokinetic Study in Rats (Sera and Liver) Laboratory Report No. FACT-TOX-145 (W2814) Requester Project No. T-7132.2 Attachment A Table o f Results - Sera Analysis 000519 02S000 n> T* 5X Laboratory Report Analytical Report of Data for PFOSA Pharmacokinetic Study in Rats (Sera and Liver) Laboratory Report No. FACT-TOX-145 (W2814) Requester Project No. T-7132.2 Attachment B Table o f Results - Liver Analysis 000521 FACT-TOX-M5 Study: Product NumberfTest Substance): Matrix. Method/Revision: Analytical Equipment System Number, instrument Software/Venion: Date of Extraction/Analyst: Date of Analysis/Analyst: Date of Data Reduction/Analyst Sample Data TOX-145 Pharmacokinetic Study ofPFOSA in Rats. T-7132.2 Rat Liver ' ETS-8-6.0 and ETS-8-7.0 Soup 020199, Amelia 062498 Masslynx 3.3 r 10/13/99,11/04/99 SEE/RWW/SAL 10/15/99,10/19/99 MMH, 11/05/99 IAS, 11/10/99 IAS 10/18/99,10/20/99,11/08/99,11/11/99 1AS/MMH Filename: R-Squared Value: Slope: Y-Intercept See Attachments See Attachments See Attachments See Attachments RAT LIVER Group Dose Sample # PFOS Calc. Cone Method Blk H20Blk-11 H20Blk-l 1 Vi 0.00 0.00 Matrix Blk H 20 Blk-2 H 20 Blk-2 RBL10199-Liver Blk-lt RBL10199-LiverBlk-ll 0.00 0.00 0.00 000 QC 250 ppb RBL10199-Liver Blk-2 RBL10199-ver Blk-2 9R03230M, Day 1-MS-11 9R03230M, Dayl -MSD-11 1 86 0.00 276 264 9R03235M, Day4-MS-12 9R03235M, Dav4-MSD-!2 226 216 9R03240M, Day29-MS-l 9R03240M. Day29-MSD-2 212 191 Group 1 0,0 mg/kg 9R03230M. Dayl 9R03231M. Dayl 0.00 0.00 9R03232M, Dayl 9RQ3233M, Dayl 9R03234M, Dayl 0.00 0.00 0 00 Group 2 0.0 mg/kg 9R03235M, Day4 9R03236M, Day4 0.00 0.00 9R03250M, Day4 295 9R03238M. Day4 9R03239M, Day4 22.0 0.00 Group 3 9R03240M, Day29 000 0.0 mg/kg 9R0324IM, Day29 9R03242M, Day29 9R03243M, Day29 9R03244M, Day29 000 0.00 0.00 0.00 Group 4 9R03245M. Dayl 23660 5.0 mg/kg 9R03246M, Dayl 9R03247M, Dayl 9R03248M, Dayl 9R03249M, Dayl 32260 36179 21200 27829 Group 5 5.0 mg/kg 9R03237M, Day4 9R032SIM, Day4 36791 32619 9R03252M, Day4 42606 9R03253M. Day4 36945 9R03254M, Day4 38268 Group 6 5.0 mg/kg 9R03255M, Day29 9R03256M, Day29 20305 20638 9R03257M. Day29 22025 9R03258M, Day29 9R03259M, Day29 26172 29867 Limit of Quantitation Limit (LOQ): PFOS 26.9 ng/g, P POSA - 11.1 ng/g Limit of Detection (LOD): PFOS 8.45 ng/g. PFOSA - 3.50 ng/g Total Amount o f PFOS VI <LOD <LOD <LOD <LOD <LOD <LOD <LOD <LOD 92H 88% 75% 72% 72% 65% <LOD <LOD <LOD <LOD <LOD <LOD <LOD 0.0295 cLOQ <LOD <LOD <LOD <LOD <LOD <LOD 23.7 32.3 36.2 21.2 27.8 36 B 32.6 42.6 369 38.3 20.3 206 22.0 262 299 Average PFOS VI <LOD <LOD <LOD CLOD 90% 73% 68% cLOD cLOQ <LOD 28.2 37.4 238 Date Entered/Analyst 10/21/99, l(y22/99,11/15/99 LAC. 11/08/99 GML Date Verified/Analyst: 11/16/99 GML RSD Std- Dev. MS/MSD RPD CLOD cLOD CLOD CLOD 5% 5% 10% cLOD cLOQ cLOD 21.7 6.12 956 3.58 173 4.12 PFOSA Total Amount Average Calc Cone ofPFOSA PFOSA Vi Vl VI 0 00 CLOD 000 CLOD CLOD 0.00 <LOD 0.00 cLOD cLOD 0.00 cLOD 0.00 cLOD cLOD 0.760 0.00 cLOD cLOD CLOD 313 104% 283 94% 99% 229 76% 215 71% 74% 352 119% 330 112% 116% 0.00 cLOD 0.00 cLOD 0.00 cLOD 00 0 cLOD 0.00 cLOD <LOD 2.35 cLOD 0.00 cLOD 22.0 0.0220 466 cLOD 0.00 cLOD <LOD 2.57 cLOD 1.72 cLOD 0.724 0.162 0.00967 cLOD CLOD cLOD <LOD 6021 6.02 7015 7.02 6239 6.24 6657 666 8811 3523 3470 8.81 695 3.52 3.47 3959 3.96 3454 4105 345 4.11 3.70 855 0.0855 175 0.175 104 0.104 142 0.142 303 0.303 0.162 PFOS 9 Perfluorooctanesul cnate PFOSA Perfluorooctanesulfonanide * Samples numbers may have been switched 3237 should be 3250. These samples may be falsely high, due to carryover from accidentally switching 3237 and 3250 GML 11/16/99 RSD Std- Dev. MS/MSD RPD cLOD cLOD cLOD cLOD 10% 7% 7% cLOD <LOD cLOD 16.0 1 11 8.28 0.307 53.0 0.0859 ETS-8-7. Excel Version 5/95 TOX-145-Uver.xls 11/30/99 9:33 AM 000522 Laboratory Report Analytical Report of Data for PFOSA Pharmacokinetic Study in Rats (Sera and Liver) Laboratory Report No. FACT-TOX-145 (W2814) Requester Project No. T-7132.2 Attachm ent C Sample Receipt 000523 1 0 /0 6 /1 9 9 9 3M ENVIRONMENTAL LABORATORY REQUEST FOR ANALYTICAL/FIELD WORK 1 LAB REQUEST NO. W2814 REQUESTOR NAME: DEANNA LUEBKER DEPARTMENT: 0227 PROJECT NO: 0010535009 DATE RECEIVED: 1 0 /0 6 /1 9 9 9 DESC: PFOSA PK STUDY IN RATS TOX-145 CONTRACT LA B (S ): EXP COMP DATE: 1 2 /3 0 /1 9 9 9 DATE COMPLETED: PROJECT LEAD: KJ HANSEN PHONE NO: 6 5 1 -7 7 8 -6 0 1 8 3M FAX NO: 6 5 1 -7 7 8 -6 1 7 6 220-2E -02,7-1374 SAMPLE DATE CODE DESCRIPTION RESULT MDL o r (95% C . I . ) 1 KJH-SPEC SPECIAL STUDY - KJH # # = UPDATED DATA v/ / /to 000524 TOX-145 SAMPLES RECEIVED Barbara A. Gramenz 10/07/99 10:08 AM ET&SS Lab 2 -3 E 0 9 Fax: 7 7 8 -6 1 7 6 To: Kan J. Ram bo/US-Corporate/3M /US@ 3M-Corporate Grant A. Paul/US-Corporate/3M /US@ 3M -Corporate Lisa A. Clem en/US-Corporate/3M /US@ 3M -Corporate Kris J. Hansen/US-Corporate/3M /US@ 3M -Corporate CC! Subject: TOX-145 SAMPLES RECEIVED On 1 0 /6 /9 9 we received 10 Liver, 10 Sera, 20 Feces and 20 Urine Samples for days 1 & 2 from 3M TOXICOLOGY. FACT- TOX -145. LAB REQUEST # W 2814. PFOSA PK Study in Rats (T -7 13 2.2 ). Samples received frozen on dry ice and have been stored in Freezer F-16 at -20+V10C. Barb \)s+, f < ,J rtcstp ? * /? /? ? Printed 10/07/99 [3M Restricted] Page 1 000^25 PFOSA PK STUDY IN RATS TOX-145 LR# W2814 DAY 1 DATE 10/5/99 Gen. MALE POST DOSE URINE ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 FECES ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 LIVER ID# 9R03230 9R03231 9R03232 9R03233 9R03234 9R03245 9R03246 9R03247 9R03248 9R03249 SERA ID# 9R03230 9R03231 9R03232 9R03233 9R03234 9R03245 9R03246 9R03247 9R03248 9R03249 DAY 2 DATE 10/6/99 Gen.MALE POST DOSE URINE ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 FECES ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 BEST COPY AVAILABLE Chain of Custody Record 3M Environmental Laboratory Form 35176 PWO 3M Facility Cc/~fiofodtC ToyT Address City. State. Zip Code 3M Project Title 3M Facility Contact 3M Telephone Number 09303 3M Rn veiqfuuseasitveir T y ta r)y \n ^ 3M Protect Lead * U /tk P x r - fiiY i/e ju J S c ta J - 3M Pioject Number ,T 0*-l46 t .T -^T Q .S- ii/eATS * ~ f 7/J&7-S?-00!O =)^ f 0 7 3M Department Numoei -- Ludb& y~ o z a 'i Lab Request/Template/4umoer (jo z u 4 Sampled By (Print) T x fiV\</YK' M t b & y ' Sameter Signature -. < M pi Item # t! Sample Description 1 D y lf& td S o iL n rfj 2 j 2 " 11 " 3 D y / fb S tm o fw L 4 D / ^ - >< >' " 5 n 'i / PoSf^oSo L o re s ' 6 P y / fS ttjj S L j 7 Contractor Date U l Date Time Matrix / f l / S IrfiM U s o \Z-J itilo lir.o C j /r / ^ ftx c S /iV 5 fa c i m /s rfy m / o f t "TpIVX Number Containers of each Preservatives O Z n O Z Z 8N X % ZZ Total Containers of Each Item Sam ples Split See Attachm ent Comments / 0 & '( n .Y t> f J G S oacjI f i r 1 U // rtvit* / ty O ' it ( ( S s ry i l P i a iA l* i f -S 9 it n D C o irv i d}o 3J30-3` h U J rr^ lty 8 9 10 11 12 13 1 ^ -------- -- _______ a ABfic-J<r * ' -------------------------------------------------------------- ------------------------ -------------------------------------------------------------------- Item # \ </' Relinquished By/Affiliation Y n /u v t U bkf Time Date l fu (4% Shipped Via / Received By/Affiliation Time Date / ^ y ~ Z C > /> /99 000527 Omqm, Acculici '*J^ See Reverse Side For Instructions TOX-145 SAMPLES RECEIVED A Barbara A. Gramenz 10/11/99 11:54 AM ET&SS Lab 2 -3 E -0 9 Fax: 7 7 8 -6 1 7 6 To: Kari J. Rambo/US-Corporate/3M/US@3M-Corporate Grant A. Paul/US-Corporate/3M/US@3M-Corporate Lisa A. Clemen/US-Corporate/3M/US@3M-Corporate Kris J. Hansen/US-Corporate/3M/US@3M-Corporate cc: Subject: TOX-145 days 3&4 SAMPLES RECEIVED On 1 0 /8 /9 9 we received 10 Liver, 10 Sera, 20 Feces and 20 Urine Samples for day 3 1 0 /7 /9 9 & day 4 1 0 /8 /9 9 from 3M TOXICOLOGY. FACT- TO X -145. LAB REQUEST # W2814. PFOSA PK Study in Rats (T-7132.2). Samples received frozen on dry ice and have been stored in Freezer F-16 at -20+V10C. Barb Printed 10/11/99 [3M Restricted] Page 1 00052 PFOSA PK STUDY IN RATS TOX-145 <LR# W28??^ DAY 3 DATE 10/7/99 Gen. MALE POST DOSE URINE ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 FECES ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 DAY 4 DATE 10/8/99 Gen.MALE POSTDOSE URINE ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 FECES ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 LIVER ID# SERA ID# 9R03235 9R03235 9R03236 9R03236 9R03237 9R03237 9R03238 9R03238 9R03239 9R03239 9R03250 9R03250 9R03251 9R03251 9R03252 9R03252 9R03253 9R03254 g)9R03254 T H e R c A R T i e o 9 R 3 2 5 4 5 6 R K SATApi_5 h b [Rs> S u t d c a Jt kjooiT) I o m i c a c w e . w g *. 000529 OCSQOt* bb|./oi b UIti lo t "^9 -* o Vi. V v itiO T fb \ 0 >**< .O S - v t \ ty nw 7 - '\ - io 'pvp^ro -v e ^ J , B W O V fO m O O C O W -Lsroa 1 1 1 9 9 9 ? ? S o y b 3 < Q ~ m g ^ ^ Q 3 w v s m ^ 9 s t ?5 e Q rH b o o a i 3 ra v f 3 3 h i frszeoy6(i) t-SZE0a6 6930a6 cszeoa6 8S30a6 zszeoa6 ZSZ0a6 Z93E0a6 l9ZS0d6 tSZE0M6 9SZE0b6 0SZE0d6 0SZE0d6 SSZ0b6 6CZC0d6 6EZE0d6 t*ZE0b6 8EZE0H6 8E3E0a6 Et'ZEOdG ZC30a6 ZZ06 3t-30a6 9EZE0d6 9EZE0d6 i^zEOb SZE0a6 SESEoae 0frZ0b6 #qi va3S #ai a3An #ai S303d 6S30a6 8S306 ZS30a6 9S3E0a6 SS3E0a6 t*ZE0b6 Et'ZEoae z^zEoae l.frZ0y6 0frZE0a6 #ai 3Nian 3SOaiSOd 31VWU90 66/8/01 31VQ PAVO 6S3E0a6 6SZE0H6 8SZE0b6 8SZE0a6 ZSZ0b6 ZSZ0a6 V5 993E0d6 SSZEObS 9SZE0a6 SSZE0a6 t^ZEOb frfZE0a6 EfrZE0b6 Et>ZE0a6 3t-30a6 Zt-ZE0a6 IV3E0H6 i^zEoae 0t>Z0b6 0frZE0a6 #ai S303d #ai 3Nian asoaisod 3*iv w u 9o 66/z/oi3va c a v o n8ZM #l Sn-XO l Siva Nl Aanis Md VSOdd BEST COPY AVAILABLE Chain of Custody Record 3M Environmental Laboratory Form 35176 - PWO 3M Facility C rfb rn C tAddress '1 0 / ' c r^ e :-o ^ City. State. Zip Code 09600 3M Project Title JfTJjSTS -p rv .K A TX 3M Facility Contact T -'J n .x T s f a t n r t O --' 3M Telephone Number 3M Requester D eciru v:^ 3M Project Lead Tow ns L u e b kti/ - " cc*J~ 3M Project Number ^ r T - n ( Q. Oo ID j iT u o 'l 3M Department Number Lab Request/Tempiate Number ----------u a f t f Sampled By (Print) O tfxn n rx iu d k /lc r ^ Sampler Signature y Contractor Date Number Containers of each Preservatives c liiy / I ^ M ^ i Item f l Sample # Description /Zs7 l . Date Time ___ Matrix > i n ozx 8 X X %z 1 j y - ? R > 9 D c > O L L r,n t- p h PPP! t.ln n C ; 2 n h fe 'e c /s / b / 7 s^fl/Y f l e t i 3 D y '1 " " L b ^ n l i f t cW i 4 ' n i> 1/ 'R e c S m i r % .e -i 5 y il P tit /-v c r / / j p a lp r*I b Y t r 6 ' " " 7 z s : r ^ r 8 Total Containers of Each Item Q Sam ples S plit See A ttachm ent Comments /P J0_ /o t-/ -7 '/ h ' fO / i / 0 * $ y# ` j & / S f r S 5- ^ (0 V ItQ 77^ 9 i, --,----- -- ____________________ 10 L n 11 12 13 ---------- Item # / - (j? Relinquished By/Affiliation P fO fi/Y t t f t k l / / Time Date itr tw Shipped Via Received By/Affiliation urbadi& u*ifi& f~ ( j/ i^ f t C h in * . / 3 / h Time Date ---H---.-o-o- pf-f-K- *----- I I dpI m 000531 Onymal Acc^n.*,<,!> , .j LAC See Reverse Side For Instructions T0X145 day 29 SAMPLES RECEIVED Barbara A. Gramenz 1 1 /0 2 /9 9 02:13 PM ET&SS Lab 2-3E-09 Fax: 778-6176 To: Kari J. Rambo/US-Corporate/3M/US@3M-Corporate Grant A. Paul/US-Corpo/ate/3M/US@3M-Corporate Lisa A. Clemen/US-Corporate/3M/US@3M-Corporate Kris J. Hansen/US-Corporate/3M/US@3M-Corporate cc: Subject: TOX-145 day 29 SAMPLES RECEIVED On 1 1 /2 /9 9 we received 10 Liver, 10 Sera Samples for day 29 from 3M TOXICOLOGY. FACT- TOX 145. LAB REQUEST # W2814. PFOSA PK Study in Rats (T-7132.2). Samples received frozen on dry ice and have been stored in Freezer F-16 at -20+V10C. Barb yi f* (Jf tt ( t --/ Printed 1 1 /0 2 /9 9 [3M Restricted] Page 1 000532 PFOSA PK STUDY IN RATS TOX-145 LR# W2814 DAY 29 DATE 11/2/99 Gen.MALE POST DOSE LIVER ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 SERA ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 000533 Chain of Custody Record 3M Environmental Laboratory Form 35176 - PWO 3M Facility C c y p Y J tc j ~ 7 ch / Address 3M Project Title P F b S ft3M Facility Contact 09305 P tC 7 -- Q lj n L 'Q . in k c/ 5 3M Requester 3M Project Lead /facLrcu ^ /a c o -S T a x ( `f i O 3/0535 O 9 3M DeMffry.nl Number City. Slate. Zip Code T / o ^ n n c^ 3M Telephone Number I a a c J o Kj l S ~ ^ 439/ la b Requestsempiale Number u m iH Sampled By (Print) V K o s iA Q ^ L u c io Sampler Signature /// Item # ( / Sample Description Contractor Date (fa L Date Time Matrix Number Containers of each Preservatives 1 Z r> o z 8N z 9 zz Z i Total Containers of Each Item Sam ples S plit See Attachm ent Comments 1 t i \ I L T y r J v 'U f fM fa / l i b f a j e > - l n c * ~ 2 R r jJ - U ^ n Z itq i/a fr c R ft '1 n 3 i& t G s Z * - ' v c h > d r (m P D I / t < S sz> ^ 4 2 f il& z u X n c ild q F h tS /9 c* i' 5 07 _s_ $ 5 6 7 8 J --------- _____ 9 //ra ____ ----------- --- - -- ' 10 11 12 13 ------------ --------- " " Item # Relinquished By/Affiliation Tim e Date Shipped Via ^B^ceived By/Affiliation Tim e Date w t-H C/t Co D C arV & U K b / 4 / T t t y i & t p h i en f r a t J S j j M c r ' / ' 3 f t ---/ -/ f--4-A** 9s Onymal Ai <oinpjiiyn ,j Sunlit. > .1I ! I- , . See Reverse Side For Instructions Laboratory Report Analytical Report of Data for PFOSA Pharmacokinetic Study in Rats (Sera and Liver) Laboratory Report No. FACT-TOX-145 (W2814) Requester Project No. T-7132.2 Attachment D Screening Results o f Dose Verification 000535 Kris J. Hansen 11/04/99 02:29 PM Tel: 7 7 8 -6 0 1 8 2 -3 E -0 9 Fax: 7 7 8 -6 1 7 6 Environmental Lab To: Andrew Seacat/US-Corporate/3M/US@3M-Corporate Deanna J. Luebker/US-Corporate/3M/US@3M-Corporate cc: Lisa A. Clemen/US-Corporate/3M/US@3M-Corporate Subject: TOX145: PFOSA PK, Dose Verification Hi Andrew and Deanna: We have completed our screen of the PFOSA dose in TWEEN. Error bars are about + /-3 0 % . PFOSA was determined in triplicate and PFOS and POAA from a single analysis. I'd classify this data as screening quality and if this data poses any major questions about the interpretation of the tox data, we may need more data points for the PFOS and POAA. However, I did check for the presence of the POAA on two different instruments. Also, in one of your voice mails, Andrew, you mentioned concern about photolysis of PFOSA to PFOS. All of the data that I've seen indicates that there may be photolysis of PFOSA to POAA (not verified yet), but there is no evidence of PFOSA photolysis to PFOS. Since the photolysis experiments were conducted under very strenuous conditions, I don't think you have much to worry about with your samples (at least not for a few dozen years!). In TWEEN 80: PFOSA 133.26% of expected dose of 1000 //g/mL recovery 130% PFOS 185% of expected dose of 10 //g/mL recovery 115% POAA recovery 121 % --> 1 3 3 0 //g/mL --> 1 8 .5 //g/mL --> 2 .5 //g/mL spike spike spike Let me know if you have questions, kjh 0003C6 Andrew Seacat 10/27/99 02:53 PM 3 M M edical Dept. Toxicology Services Andrew M . Seacat Ph.D. 3M Center 220-2E -0 2 Saint Paul, M N 5 5 1 4 4 Tel: (6 5 1 )5 7 5 -3 1 6 1 Fax: (6 5 1 )7 3 3 -1 7 7 3 To: Kris J. Hansen/US-Corporate/3M/US@3M-Corporate cc: Fred L. DeRoos/US-Corporate/3M/US@3M-Corporate Deanna J. Luebker/US-Corporate/3M/US@3M-Corporate Sue Chang/US-Corporate/3M/US@3M-Corporate Subject: PFOSA dosing solution Kris, As we were discussing in our last Friday's meeting,we would like to have the PFOSA dosing solution checked for PFOSA concentration, and for PFOS and PFOA, which may under certain conditions arise from photolysis. We left the dosing solution with you. I understand there is a problem with the Tween 80 concentraton being too high to allow sufficient dilution for analysis of some PFOS concentrations. Given that the starting material has approxmately 1% PFOS in it could the dosing solution sample be analysed to see if there is significantly more PFOS in there? If not possible, then perhaps we could ask Fred Deroos to analyze the dosing solution? The dosing solution was prepared as follows: Stock PFOSA in acetone was made up at 52mg PFOSA/O.52 mL acetone = 100 mg/mL This was diluted into 5 1.48 ml of 2% Tween 80 to acheive the dosing solution: Final concentration of PFOSA = 1mg/ml Final cone of acetone = 1% Final cone Tween 8 0 = "2% Thanks, Andrew I* /VO vu /' U IT '7 Jw `Tt TOX145 Twoes tO- D o s tC n T m liM Study Date Analyzed File # Instrument POAA Sample ID Tween dose-NA TOXI45 11/2/99 110299a Soup 020199 Dose c o a c (ppb) - , Expected Dose (ppb) Amt o f spike (ppb) Dose + MS cone, (ppb) % Recovery o f Dose _______ 1 NA 204 29 48 #VALUEi % Recovery o f MS Date o f Extraction 121 11/2/99 PFOS Sample ID Tween dosc-20ppb Dose c o a c (ppb) Expected Dose (ppb) Amt o f spike (ppb) Dose * MS c o a c (ppb) % Recovery o f Dose % Recovery o f MS Date o f Extraction 369 200 207 i 56 08 ) MS 11/2/99 fKPH ruflu I (o 4 . n r & * * * ;~ T w e E '4 PF os i-Tw ie^M = ) lO p p ^ v f- 2 0 b = 9 * ^ 'PvJWA ,p 4. V f f b f** po* 2 -4 pr*' 4 -? M / / HvyyL' 5^0 t* \U "2-5" y j j 0C 0538 Study Date Analyzed File# Instrument TOX145 10/29/99 102999a Soup 020199 PFO SA in 2% Tween 80, Sample TN-A-3046 File # 10299013 10299014 10299017 % Recovery of Dose Recovery of Dose amt (ppb) 132.64 265.27 134.31 132.83 268.62 265.65 Mean Standard Dev. %RSD 133.26 0.917 0.688 266.51 1.83 0.688 y t ce PfbiA **> * ^00539 PFOSA dosing solution Andrew Seacat 10/27/99 02:53 PM 3 M Medical Dept. Toxicology Services A ndrew M . Seacat Ph.D. 3 M Center 22 0-2E -0 2 Saint Paul, M N 5 5 1 4 4 Tel: (6 51) 5 7 5-31 61 Fax: (6 51) 7 3 3 -1 7 7 3 To: Kris J. Hansen/US-Corporate/3M/US@3M-Corporate cc: Fred L. DeRoos/US-Corporate/3M/US@3M-Corporate Deanna J. Luebker/US-Corporate/3M/US@3M-Corporate Sue Chang/US-Corporate/3M/US@3M-Corporate Subject: PFOSA dosing solution Kris, As we were discussing in our last Friday's meeting,we would like to have the PFOSA dosing solution checked for PFOSA concentration, and for PFOS and PFOA, which may under certain conditions arise from photolysis. We left the dosing solution with you. I understand there is a problem with the Tween 80 concentraton being too high to allow sufficient dilution for analysis of some PFOS concentrations. Given that the starting material has approxmately 1% PFOS in it could the dosing solution sample be analysed to see if there is significantly more PFOS in there? If not possible, then perhaps we could ask Fred Deroos to analyze the dosing solution? The dosing solution was prepared as follows: Stock PFOSA in acetone was made up at 52mg PFOSA/O.52 mL acetone = 1 0 0 mg/mL This was diluted into 51.48 ml of 2% Tween 80 to acheive the dosing solution: Final concentration of PFOSA = 1mg/ml Final cone of acetone = 1 % Final cone Tween 80 = "2% Thanks, Andrew j /"6 00 o . o7Sj k L~ ^ ==- 'firbS Co*-C . /Off*, * ~ ooo 9*- Printed 11 /04/99 [3M Restricted] 2-mt- /OOO^Ci |# a g e 1 00054 TOXI4S Tween IO- Dose Coniinnstiofi Study Date Analyzed File # Instniment POAA Sim ple ID Tween dose-2ppb TOXI45 10/29/99 102999a Soup 020199 Dose cene, (ppb) Expected Dose (ppb) A n t o f spike (ppb) Dose + MS cone, (p % Recovery of,QPh % Recovery o f M Opte o f Extraction ______ t a1 67 200 204 3.51 ; ( 9o ' 10/29/99 PFOS Sample ID Tween dose-2ppb Dose cone (ppb) Expected Dose (ppb) Amt o f spike (ppb) Dose + MS cone, (p % Recovery o f Qp. % Recovery o (ft| Date o f Extraction 4.13 2.00 2 07 6 4 0 ___________ M t l ' 10 J 10/29/99 PFOSA /.' s o b o ?? A * M i'* cAm m / : SVD i (Q <> o* f'.^SOO (eth'c* pepavi JSJL - % fi W VfS / P O A Jds-f y -ir T O f f b S p (a(M \e> It O Q l) Date Data Analyst: "//A? 3as FACT: DATA REVIEW SUMMARY FORM Data Review Sign-Off Analyst Review Name / Date: j. 7 o*-i>fs "TUcla. fo Technical Review Name / Date:____ ijh \ u \ m Sample List: Set-up Analysis Date/Analyst: 102111. f3f t i h i j* * Quality Assurance Review Name / Date:____________ Data Entry:. Instrument: ______________ Comments / Justifications: Analyte: Q ~P>AA Cch f ) (Acceptable Linear Range: LOQ:--- i'bQppi RA2- Calibration Checks: OF- - MS/MSD: Data Status: > /0>pj>L E xtraction Blank: / / f t Matrix Blank: AW ~--/ 4 Analyte: 'Pfa'S C<-H') [Acceptable Linear Range: ! LOQ:. R -2 : _ 9U?3S ^ Extracted Blank: //A Matrix Blank: hr__ jx **-4 s kj<e <fJur/ueet/ Ir* * - 4Ll Cuy-t/e t*~ O f c__ I* C u S ~ >n- 4 U ________ louer Ji Jx>)rd* L ftri C o t i . c e 4 a IX-___ ~f F9 \td^LS o / / s i 4L.. 0 ?T __CfreJ<r `7^.*. ~ 3 % -f* -r 4 l I u/es f '3 a S %A? So**- Cc-itfU'i'M.r' Ust-S K ^ i^ c f /- AOff mJ. - "/or/ff_________ Tu f -- fjda i Calibration Checks: K - />s /*. Z S ^,,b c * /d tc \ kyhr y *- VaJuCS / ess. MS/MSD: Data Status: 0 -1?__a-^tJ J t vud**`L* ___ 4U . +30*/ 4L LlabJ**' Co/tc . Analyte: T Y sgX w Acceptable Linear Range: LO Q : UJOrd R"2: O - l f f l C f ir Extracted Blank:_____ Matrix Blank: M A Calibration Checks: 6 k . - c d c L c L = -----1 t- MS/MSD:___________ ___ __________________________ ________ Data Satus: /L fc S t t * - l n u - c / / , 7 ^ . u o t f g l k s . ~~~J S ''l l / f t ____________________ Ak^/ili foi}tpi S'.o-*SJ ^fsriSr (y^BC-eef ih* o r A c u .r 4 c kflc~^KUA y '*o*t-eC.. CC iu'.-rs'ltK*e. *sf& . AwtJwis J ~/U /.3/yX 4^ JS.03[j 000542 Dale Data Analyst: U P 'IK FACT: DATA REVIEW SUMMARY FORM 3*s Data Review Sign-OfT Analyst Review Name / Dale: /, * M /tf ^ zJ z- FACT Study #: Matrix/Timepoints: X e ^ b <7^sir C*x-u S a^-pljL 1 * 1 J u l M U I Sample List: Set-up Analysis Date/Analyst: lo ? t f l <t_ ^ l h 7a 5 Quality Assurance Review Name / Date:____________ Data Entry:. Instrument: r, W Analyte: X s ( Tc f f U) ^ Acceptable Linear Range: //A LOO: AM RA2: / / ?? Extraction Blanlc AM Matrix Blank: H A Comments / Justifications: ______________________ _G__)______ J`nu~-k tet-re/. / ___ /> ujuu*- kic, -dia- y > - / f ^ ~'^3* s CwUiVyo/to'' A-g-S k-die*crf //t_ Calibration Cheeks: MS/MSD: Data Status: a/a T T srp A fta, Coums L*-fie.cl aj/^oic-i dl* Pcvudl** Luck, is as */* as foioas JS ' 'b * 00054o I <*01 or* & ? H* E 8 o O O o 1 V lOppb- 9/10/99 RWW oooooooc tOK) K) t SOSOSOs. 5 0 0 0 0 0 0 C JOODOOOOOOOOC * tKol tKo>ttUe K) tOvNoI ut. J WM WN IO WIJ IOWWW h S^SOSOSOSOSOSOSOSOSOSDSOSOSOSOSOSOIOSOSI JOOOOOOOOOOOOOOOOOOOC J<NO)'PC*(PD*'PJ` fPf*lPU*<P^U- iPK*)Ml-P>*OP^C- 00^000l0U0I0(>0U0MC 1]1)1]-flu >flh) >I|<<5 sssssasss? 13 !X 3 X SSgSSSSSSQSSSSSSI P- P ' p - p - H- P - p - p - p - 9 X H' H H a V- H- h P- P P- K K t - i s f l XXXXXXXXX i i i i i i t it oo Xi *u*i u*i en >Xi XXiXX iX iX iX <X m ce P* P* SO I I o 03 oooooooo CD CO GO 03 00 00 OO 00 je so o *o o nj nj Ooo O iM/ltl t> > r w o'D X O'fl'TJ 00 o O <7i VI V) 'o x ix iio x iiA v x x o rK ooooooooo COODCDOOCDCSCOCOCO OiOtffiVOiOiOiOiOi 'H ' m n >O (>(i M 1 Ul *OI 3 UlO O J1O O t) 3 *3 13 U 13 33r11c33rtTciJr*C3<TnCTuCT cr er I I I I )lOU)Nosso. O IOSNNHH sNSHH HO O aOO's.'-.v.iOM o so so so so so ya I iii !I muoio33<t3anl> S33 er ai* aa aa p"C o o *0 o ^ trs SK)hO so i SO 13 NI er JU IM H U IK IPU IH - soouiotfl oo coor i1ta3r o twc)r 1Tct33=r1c3_0r1tt>3r1*to3r1ct3rc13r lili so so SOSOSOSO v ^ H OOOO'-.-^.'-.lOsO NXSS.SOSOSOSOSO SOsOso sOSOso SO so so so so ya ja I ii ii nH c0 ikrAkAr nk pa- cr frpt1hf6a rt o o p - Va &a &g ? l&*r 3o ?3!? a p' **^ ;ir*? tso Os M O H .t.o eo w e0 P*13 w13 ss o3 013 to o 88 p* 3 "S uinii)(nvitii(i)ii) a ao.o5.oa. a5 aa &5 oo. p.p.p.p.p.p.p.(s UIKIH O U iauiK IH M H O O U IO U IH a a a a a a a a arAfrfrktArktrgtirtprifArrSrtr fS A. ft. p- f\. p. p. p. p. CU aaaaaaaaa '1 Msi HU MH HO sHj POl pH slO O lO O O SSO P P* p* NI OS SP OH i -I'O-o -o -j -o -j -j -j -j -o -o P*P*P*P` P*P` 0 0 P P * 0 WUIOKIOPttQXnOKIOO IPKIsllOUlUJOsJMPSOI f> K) p* K-*i Uu>otO O 0>O i^n Kl Msj U p PU OsS| PSJ SBmSSg K> U> uo>s p H p* N ?11 M Ul fc SOO Ul to Ul KUl) 000SO0 tO P* p* O00UUll M os &5i3&&m?g:SS XXX s trn tr p * PW OUIM P C o lJp w ff iO O s O nIOUMOIs OS-JP U'JM M UIPfJUI OO SOOs -O si p o NI Ul UlOl AM- KO sO PIM P O P W O islO iP O O P WUSOSSOsIPMKI KipsjKJsim ote tJ M I ts) tO | COslOKIffiffiOWsJ OS r= ro to *< \A Standard 752.00 7.129 5411 bbX 538 'V, Quantify Compound Summary Report T0X145-tween 60 doae confirmation for POXA, pros, 6 POAA- axt. 10/29/99 iaa Sample List: C:\MASSLYNX\eoup02Q199.pro\8anpleDB\102999a Laat modified: rri Oct 29 10:23:59 1999 Method: C : \MASSLYNX\soup020199.pro\HethDB\102999a Last modified: Mon Nov 01 06:21:40 1999 Job Code: Printed: Mon Nov 01 06:47:34 1999 Compound 2: pros (Ch2) Name 1 102999001 2 102999002 3 102999003 4 102999004 5 102999005 6 102999006 7 102999007 8 102999008 9 102999009 10 1Q2999Q10 11 102999011 12 102999012 13 102999013 14 102999014 15 102999015 16 102999016 17 102999017 18 102999018 19 102999019 20 102999020 21 102999021 22 102999022 23 102999023 24 102999024 25 102999025 26 102999026 27 102999027 28 102999028 29 102999029 Samplalist Text MeOK Blk MeOH Blk FCMix-99086-43 -1, lppb- 9/10/99 RWW FCMix-99086-43 -2, 5ppb- 9/10/99 RWW FCMix-99086-43-3, lOppb- 9/10/99 RWW FCMix-9908 6-4 3-4, 25ppb- 9/10/99 RWW FCMix-99086-43-5, 50ppb- 9/10/99 RWW FCMix-99 086-4 3-6, lOOppb- 9/10/99 RWW FCMix-99086-43-7, 2S0ppb- 9/10/99 RWW FCMix-99086-43-8, SOOppb- 9/10/99 RWW FCMix-99086-43-9, 750ppb- 9/10/99 RWW MeOH Blk T0X145-PFOS/POAA in Tveen-dose-2ppb- 10/29/99 IAS TOX145-PFOS/POAA in Tveen-ms-4ppb- 10/29/99 IAS FCMix-99086-43-4, 25ppb- 9/10/99 RWW MeOH Blk TOX145-PFOSA in Tween-dose-200ppb- 10/29/99 IAS TOX145-PFOSA in Tween-aus-300ppb- 10/29/99 IAS FCMix-99086-43-7, 250ppb- 9/10/99 RWW MeOH Blk FCMix-99086-43-1, lppb- 9/10/99 RWW FCMix-99086-43-2, 5ppb- 9/10/99 RWW FCMix-99086-43-3, lOppb- 9/10/99 RWW FCMix-99086-43-4, 25ppb- 9/10/99 RWW FCMix-99086-43-5. 50ppb- 9/10/99 RWW FCMix-99086-43-6, lOOppb- 9/10/99 RWW FCMix-9908 6-43-7 , 250ppb- 9/10/99 RWW FCMix-99086-43-8, SOOppb- 9/10/99 RWW FCMix-990 86-43-9. 750ppb- 9/10/99 RWW Type Standard Standard Standard Standard Standard Standard Standard Standard Standard QC QC Standard Standard Standard Standard Standard Standard Standard Standard Standard Std Cone 1.01 5.03 10.00 25.20 50.30 101.00 252.00 503.00 755.00 25.20 252.00 1.01 5.03 10.00 25.20 50.30 101.00 252.00 503.00 755.00 RT 7.315 7.295 7.226 7.291 7.240 7.266 7.248 7.246 7.272 7.265 7.289 7.309 7.313 7.340 7.331 7.338 7.314 7.321 7.313 7.295 7.272 7.330 7.335 7.342 7.291 7.313 7.363 7.314 7.291 Area Flags 202 bb 42 bb 148 MM 476 MM 913 MM 2108 bb 4162 bd 8473 bd 22878 bbX 41708 bbX 56477 bbX 170 MM 424 bb 619 bb 2284 bb 63 KM 373 MM 398 MM 22863 bb 91 bb 158 bb 530 bb 989 bb 2289 bb 4761 bb 8949 bb 22364 bbX 42068 bbX 55508 bbX Cone. *Dev 1.56 0.00 0.93 -8 4.74 -6 9-81 -2 23.71 -6 47.57 -5 97.67 -3 265.05 5 483.87 -4 655.48 -13 1.18 4.13 6.40 25.75 2 0.00 3.55 3.63 264.88 5 0.27 1.04 3 5.37 7 10.70 7 25.80 2 54.53 8 103.19 2 2S9.08 3 488.05 -3 645.14 -15 Paso 2 Soup 020199 : Quantitt! and printad by- iaa on 11/01/99 000545 Quantify compound Sunnary Report TOX145-tween BO dosa confirmation for POAA, pros, 6 POAA- axt. 10/29/99 las Sample List: Last modifiad: Method: Last modifiad: Job Coda : C:\MRSSLYMX\soup020199.pro\BaavlaDB\102999a Fri Oct 29 10:23:59 1999 C:\MAS6LYNX\*oup020199-pro\HathDB\102999a Mon Nov 01 06:21:40 1999 Printed: Mon Nov 01 06:47:34 1999 Compound 3: PFOSA <Ch3) Name 1 102999001 2 102999002 3 102999003 4 102999004 5 102999005 6 102999006 7 102999007 3 102999008 9 1C29990Q9 10 102999010 11 102999011 12 102999012 13 102999013 14 102999014 15 102999015 16 102999016 17 102999017 IS 102999018 19 102999019 20 102999020 21 102999021 22 102999022 23 102999023 24 102999024 25 102999025 26 102999026 27 102999027 23 102999028 29 102999029 Samplelist Text MeOH Blk MeOH Blk FCMix-99086-43-1, lppb- 9/10/99 RWW FCMix-99086-43-2, 5ppb- 9/10/99 RWW FCMix-99086-43-3, lOppb- 9/10/99 RWW FCMix-99086-43-4, 25ppb- 9/10/99 RWW FCMix-99086-43-5, 50ppb- 9/10/99 RWW FCMix-99086-43-6, lOOppb- 9/10/99 RWW FCMix-99086-43-7, 2S0ppb- 9/10/99 RWW FCMix-99086-43-6, SOOppb- 9/10/99 RWW FCMix-99086-43-9, 750ppb- 9/10/99 RWW MeOH Blk TOX145-PFOS/POAA in Tveen-dose-2ppb- 10/29/99 IAS TOX145-PFOS/POAA in Tween-ms-4ppb- 10/29/99 IAS FCMix-99086-43-4, 25ppb- 9/10/99 RWW MeOH Blk TOX145-PFOSA in Tween-dose-200ppb- 10/29/99 IAS TOX145-PFOSA in Tween-ms-300ppb- 10/29/99 IAS FCMix-99086-43-7, 250ppb- 9/10/99 RWW MeOH Blk FCMix-99086-43-1, lppb- 9/10/99 RWW FCMix-99086-43-2, Sppb- 9/10/99 RWW FCMix-99086-43-3, lOppb- 9/10/99 RWW FCMix-99086-43-4, 25ppb- 9/10/99 RWW FCMix-99086-43-5, 50ppb- 9/10/99 RWW FCMix-99086-43-6, lOOppb- 9/10/99 RWW FCMix-99086-43-7, 250ppb- 9/10/99 RWW FCMix-99086-43-8, SOOppb- 9/10/99 RWW FCMix-99086-43-9. 7S0ppb- 9/10/99 RWW Type Standard Standard Standard Standard Standard Standard Standard Standard Standard QC QC Standard Standard Standard Standard Standard Standard Standard Standard Standard Std Cone 1.01 5.03 10.10 25.10 50.30 101.00 251.00 503.00 754.00 25.10 251.00 1.01 5.03 10.10 25.10 50.30 101.00 251.00 503.00 754.00 RT 7.833 7.790 7.741 7.809 7.803 7.805 7.766 7.809 7.857 7.895 7.941 7.982 7.920 7.969 7.984 7.989 7.943 7.950 7.964 7.990 7.947 8.003 7.988 7.948 7.942 7.965 7.992 7.989 7.917 Area Flags 18209 MM 835 MM 1102 MMX 1881 MMX 2710 MM 6408 MM 10741 MM 21634 MM 68915 MM 139095 MM 199487 MM 2140 MM 72407 bb 73318 bb 8797 MM 596 KM 72510 bd 105109 db 75327 MM 870 MM 783 MMX 1994 MMX 3433 MM 8204 MM 14786 MM 30309 MM 76998 MM 140797 MM 201774 MM Cone. XDev 66.15 2.32 3.30 227 6.16 23 9.21 -9 22.80 -9 38.71 -23 78.74 -22 252.44 1 510.28 1 732.15 -3 7.12 265.27 268.62 31.57 26 1.44 265.65 385.42 276.00 10 2.45 2.13 111 6.58 31 11.87 17 29.39 17 53.58 7 110.61 10 282.14 12 516.53 3 740.56 -2 Paga 3 Soup 020199: Quantitated and printed by ias on 11/01/99 Quantify Compound Surnnary Report TOX145-tween 80 doss confirmation for POAA, Pros, & PQAA- xt. 10/29/99 ins Sample List: C: \MASSLTOX\soup020199 .pro\8anc>leDB\102999a Last modified: Pri Oct 29 10:23:59 1999 Method: C:\MASSLYKX\soup020199.pro\MethDBU02999a Last modified: Mon Nov 01 06:21:40 1999 Job Code: Printed: Mon Nov 01 06:47:34 1999 Compound 4: IS <Ch4) Name 1 102999001 2 102999002 3 102999003 4 102999004 5 102999005 6 102999006 7 102999007 a 102999008 9 102999009 10 102999010 11 102999011 12 102999012 13 102999013 14 102999014 15 102999015 16 102999016 17 102999017 18 102999018 19 102999019 20 102999020 21 102999021 22 102999022 23 102999023 24 102999024 25 102999025 26 102999026 27 102999027 28 102999023 29 102999029 Semplelist Text MeOH Blk MeOH Blk FCMix-99086-43-1 lppb- 9/10/99 RWW FCMix-99086-43-2, 5ppb- 9/10/99 RWW FCMix-99086-43-3, lOppb- 9/10/99 RWW FCMix-99086-43-4, 2Sppb- 9/10/99 RWW FCMix-9 9086-43-5, SOppb- 9/10/99 RWW FCMix-99086-43-6, lOOppb- 9/10/99 RWW FCMix-99086-43-7, 2S0ppb- 9/10/99 RWW FCMix-99086-43 -8, 50Qppb- 9/10/99 RWW FCMix-99086-43 -9, 750ppb- 9/10/99 RWW MeOH Blk TOX145-PFOS/POAA in Tween-dose-2ppb- 10/29/99 IAS TOX145-PFOS/POAA in Tween-ms-4ppb- 10/29/99 IAS FCMix-99086-43-4, 25ppb- 9/10/99 RWW MeOH Blk TOX145-PFOSA in Tween-dose-200ppb- 10/29/99 IAS TOX145-PFOSA in Tween-ms-300ppb- 10/29/99 IAS FCMix-99086-43- 7 , 250ppb- 9/10/99 RWW MeOH Blk FCMix-99086-43-1, lppb- 9/10/99 RWW FCMix-99086-43-2, 5ppb- 9/10/99 RWW FCMix-99086-43-3, lOppb- 9/10/99 RWW FCMix-99086-43-4, 25ppb- 9/10/99 RWW FCMix-99086-43-5, SOppb- 9/10/99 RWW FCMix-99086-43-6, lOOppb- 9/10/99 RWW FCMix-99086-43-7 , 250ppb- 9/10/99 RWW FCMix-99086-43-8, SOOppb- 9/10/99 RWW FCMix-99086-43-9 , 750ppb- 9/10/99 RWW Type Standard Standard Standard Standard Standard Standard Standard Standard Standard QC QC Standard Standard Standard Standard Standard Standard Standard Standard Standard Std Cone 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 RT 7.170 7.082 7.147 7.095 7.099 7.104 7.101 7.128 7.120 7.145 7.169 7.150 7.163 7.147 7.154 7.146 7.127 7.163 7.168 7.174 7.145 7.147 7.174 7.146 7.146 Area Flags 15 bb 4292 bb 4289 bb 4424 bb 4486 bb 4446 bb 4093 bb 2630 bb 1993 bb 1842 bb 2613 bb 1041 bb 2305 bb 2529 bb 1016 bb 1991 bb 2320 bb 2361 bb 2396 bb 2274 bb 2435 bb 2181 bb 2059 bb 1934 bb 1818 bb Cone. %oev 0.01 -99 1.48 1.48 1.52 1.54 1.53 1.41 0.91 0.69 0.63 48 46 52 54 53 41 -9 -31 -37 0.90 -10 0.36 -64 0.79 -21 0.87 -13 0.35 -65 0.69 -31 0.80 0.81 0.83 0.78 0.84 0.75 0.71 0.67 0.63 -20 -19 -17 -22 -16 -25 -29 -33 -37 Pag 4 Soup 020199: Quantitated and printed by ias on 11/01/99 000547 Method Report Method file: Last modified: Compound: Printed: C:\MASSLYNX\soup020199.pro\MethDB\l02999a.mdb Mon Nov 01 06:21:40 1999 1: PCAA (Chi) Mon Nov 01 07:36:09 1999 Compound Name: Internal Ref.: Quantify Trace: Cone. of Standards: User RF Value: User Peak Factor: Integrate Window Factor: Chromatogram mass window: POAA (Chi) [None] TIC Cone. A 1.000000. Disabled 1.000000 2.000 l.OOOODa Retention Time (mins): Relative Retention Time: RT Reference: Time Window (mins): Peak Selection: 7.173, Enabled 0.000, Disabled [None] 0.312 Nearest Response Type: Response: External Areas Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Linear Exclude 1/X None Units: Peak-to-peak amplitude: 90 Smooching: Window size (scans): Number of smooths: Smoothing method: Enabled 2 1 Join valley threshold: Reduce peak tailing: Raise baseline maximum: 30.00 200.00 5.00 Draw vertical threshold: Detect shoulders: Shoulder threshold: 90.00 Disabled 30.00 Relative height: Absolute height: Relative area: Absolute area: 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled "///*? r / / / Page 1 000548 Method Report Method file: Last modified: Compound: Printed: C: \HASSLYNX\soup020199 .pro\MethDBU02999a.mdb Mon Nov 01 06:21:40 1999 2: PFOS {Ch2) Mon Nov 01 07:36:09 1999 Compound Name: Internal Ref.: Quantify Trace: Cone, of Standards: User RF Value: User Peak Factor: Integrate Window Factor: Chromatogram mass window: PFOS (Ch2) (None) TIC Cone. B 1.000000. Disabled 1.000000 2.000 l.OOOODa Retention Time (mins): Relative Retention Time: RT Reference: Time Window (mins): Peak Selection: 7.434. Enabled 0.000, Disabled (None) 0.345 Nearest Response Type: Response: External Areas Polynomial Type.Point of Origin: Fit Weighting: Axis Transformation: Linear Exclude 1/X None Units: Peak-co-peak amplitude: 88 Smoothing: Window size (scans): Number of smooths: Smoothing method: Enabled 2 1 Join valley threshold: Reduce peak tailing: Raise baseline maximum: 30.00 200.00 5.00 Draw vertical threshold: Detect shoulders: Shoulder threshold: 90.00 Disabled 30.00 Relative height: Absolute height; Relative area: Absolute area: 1.S0, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled Page 2 000549 ( Quantify Calibration Report TOX145-tween 80 doaa confirmation for POAA, PROS, St POAA- ext. 10/29/99 las XU j- A // ' Pag* 1 Soup 020199: Quantitated and printed b y las on 11/01/99 000550 Quantify Calibration Raport TOXl45-twaan 80 do confirmation for POAA, PFOS, POJLA- axt. 10/29/99 iaa Pag 2 Boup 020199: Quantitatad and printad by iaa on 11/01/99 000551 Quantify Calibration Report TOXliS-tween 80 dose confirmation for POAA, pros, ft POAA- ext. 10/29/99 las Pag* 3 Soup 020199: Quantitated and printed toy iaa on 11/01/99 0005S2 Quantify Calibration Raport TOX145-twn 60 do confirmation for POAA, PFOS, k POAA- xt. 10/29/99 iaa Pag 4 $8653 L aboratoiy Report Analytical Report of Data for PFOSA Pharmacokinetic Study in Rats (Sera and Liver) Laboratory Report No. FACT-TOX-145 (W2814) Requester Project No. T-7132.2 Attachment E Extraction and Analytical Data 000554 Extraction Worksheet ETS-8-6.0 Study Surrogate Std M a t r i x '^ LiUc^ Approx, ppm Box# 2,,,, 1 `J-Aocs Actual ppm WK/Dav l *y #qfto8vii-u DateSpiked/Analyst ,n-t RBL10139-250ppb-CCV-11-1 to4 5 uL 9RQ3230M.Dy1.Control-250ppb-MS/D11 5 uL 9R03235M.Dy4,Control.250ppb-MS/012 5 uL RBL10139-H2Oblk-11412 5 uL RBL10139-Liver blk-11&12 5 uL RBL10139-5ppb-11412 5 uL RBL10139-10ppb-11412 5 uL RBL10139-25ppb-11412 5 uL RBL10139-50ppb-11412 5 uL RBL10139-100ppb-11412 5 uL RBL10139-250ppb-11412 5 uL RBL10139-500ppb-11412 5 uL RBL10139-750ppb-11412 5 uL RBL10139-1000ppb-11412 5 uL 9R03230M,Dy1.Control 5 uL 9R03231M.Dy1,Control 5 uL 9R03232M.Dy1,Control 5 uL 9R03233M.Dy1.Contrai 5 uL 9R 03234M ,D y1.C ontrol 5 uL 9R 03245M ,D y1.5m g/kg 5 uL 9R 03246M ,D y1,5m g/kg 5 uL 9R 03247M ,D y1,5m g/kg 5 uL 9R 03248M ,D y1,5m g/kg 5 uL 9R 03249M ,D y1,5m g/kg 5 uL 9R 03235M ,D y4,C ontrol 5 uL 9R 03236M ,D y4,C ontrol 5 uL 9R 03237M ,D y4,C ontrol 5 uL 9R 03238M ,D y4,C ontrol 5 uL FC Mix FC Mix FC Mix Comments Verified By approx.0.5 ppm approx.5 ppm approx.50 ppm actual ppm actual ppm actual ppm # 9*c>SL>-i 11 /C/v ? '/ f / c 10 uL - TL - lo /l- K/U s - tV A - - 10 uL - -- - --- 2 uL - - 4 uL - - 10 uL - - 20 uL - - 40 uL - - - 10 uL - - 20 uL - ! - 30 uL - - - 4 uL -- -- ---- ----- >^ . ra u . ioi\s _A ZJ ZJ -- -- - -- - --- --- --- --- - - - >/ B l a n k Std# ^ amount = l o ml f i J u * g/ml i Liver Extraction Method ETS-8-6.0 Date & Initials Vortex 15 Sec. Pipette Matrix, spike with appropriate surrogate or FC-Mix Volume / O ml i o - i V f v / . f t ___ | > Pioette 1 ml of 0.5 M TBA. oH 10. dH= 0 /o /3` 9 f S < ^ Std. # 990&(s~ Pipette 2 ml of 0.25 M Na2CC>3/0.25 M NaHC03buffer Std. # 'iioiQ - w - o f IP 5 IIIH ' Dispense 5 ml of methyl-t-butyl ether Shake 20 min Centrifuge 20-25 min. TN-A-^W v Shaker speed: 3oo__ Centrifuge speed: 3TOO __ 7 " __and___ Remove a 4 ml aliquat of organic layer Put on Nitrogen Evaporator to dryness Temperature: Room Temp. . Add methanol Volume J O ml TN-A- O m r //>./i/-4 S /w Vortex 30 sec. j a=T Filter using a 3cc B-D syringe with a 0.2 um filter into an autosampler vial Jj ix k tc ^ - -A>Jl o+p$B, ^>i fiV - 1 ' 3<~nt o ( iCDorpb *I l u w > adtci Rr >ph . ^ i S b f r h A w ' > ^ <-lrvL H I" C r^.L. i 1>t lOOO^S Uuv <LO^C<-V H . io 10/12/99 Draft Attachm ent A ETS-8-6.0 Extraction of P F O S from Liver Form Com pletion t / Verified By 000555 Extraction Worksheet ETS-8-6.0 S tu d v # T O X -iH J ' M a trix 'H a i Box# W K /D av Ii D a te S p ik e d /A n a ly s t 9 R 0 3 2 3 9 M , Dy4.C ontrol 9R 032S 0M .D y4.5m g/kg 9R 03251M .D y4.5m g/kg 9R 03252M .D y4.5m g/kg 9R 03 2 5 3 M , Dy4,5m g/kg 9R 03254M .D y4.5m g/kg Surrogate Std Approx, ppm Actual ppm # to-U 5 L 5 uL 5 uL 5 uL 5 uL 5 uL - - FC Mix FC Mix FC Mix Com m ents Verified By approx.0.5 ppm approx.5 ppm approx.50 ppm actual ppm # AV actual # \tr ppm actual ppm # \SJ tl\# - - - lOti-ft/c*' - - - ( ._ . 1 , - -/ - -/ - -/ -- ------------- -------------- -- - - - -- -- -- -- -, . ._... - - -_ ;------ - B la n k -'7 ? ^ ^ '/. .Vcv- Std# W o z to -u -s - Liver Extraction Method__ ETS-8-6.0 \Or /> -^ - - -- -------- =------- -------- ----- --- --------- - am ount = / cj 2!___ o - t x g/m l Date & Initials Vortex 15 Sec. Pipette M atrix, spike with appropriate surrogate or FC -M ix Volum e /. O ml P ipette 1 ml o f 0 .5 M TBA, pH 10. dH= /d /.- Pipette 2 ml of 0 .2 5 M Na,CO :s/0.25 M N a H C 0 3 buffer std. # 4 * 5 <v-i Dispense 5 ml o f methyl-t-butyl ether S hake 2 0 min C entrifuge 2 0 -2 5 min. R em ove a 4 ml aliquat of organic layer T N -A -j& i Shaker speed:_2o o C entrifuqe speed: 3TDo ____ LI ____ | Put on Nitrogen Evaporator to dryness Temperature: Room Tem D. Add methanol V o lu m e / O ml TN-A-3< W r Vortex 30 sec. Filter using a 3c c B -D syringe with a 0 .2 urn filter into an a u to s am p ler vial J U ' 0 v 3- f t ______ i o - N - m * * ' ___ / yjy __ 11 ____ 10/12/99 Draft Attachm ent A ETS -8-6.0 Extraction of P FO S from Liver Form Comi V erified By. 000556 Sample W eights/ Volumes TVlrvfc^ lO^IV'5 S ts' PrepDate(s): 10-12-99 Analyst(s): SEE Sample Matrix: Rat Liver Method/Revision: ETS-8-6.0 Target Analyte(s): PFOS, PFOSA Sample ID 9R03230M.Dyl, Control 9R03231M.Dyl,Control 9R03232M,Dyl.Control 9R03233M,Dyl,Control 9R03234M,Dyl,Control 9R03245M,Dy 1,5mg/kg 9R03246M,Dy 1,5mg/kg 9R03247M,Dy 1,5mg/kg 9R03248M,Dy 1,5mg/kg 9R03249M,Dyl,5mg/kg 9R03235M,Dy4,Control 9R03236M,Dy4,Control 9R03237M,Dy4,Control 9R03238M,Dy4,Control 9R03239M,Dy4,Control 9R03250M,Dy4,5mg/kg 9R03251M,Dy4,5mg/kg 9R03252M,Dy4,5mg/kg 9R03253M,Dy4,5mg/kg 9R03254M,Dy4,5mg/kg ______ ................ ...................- Study Number: TOX-145 Equipment Number: 0222-0900 Final Solvent St TN Number: MeOH / TN-A-2945 Matrix Blank/Identifier: Rabbit Liver Box: 99-200 Initial Weight grams Homogenized By: Verified By: Comments 0 -lli.^1 t-o/r<\ / . 0060 \ Used for MS/D 11 \ _______t lti___________ 0. 1113 .tu n i-on i l.OOTV -L MJU+ l o f t l / t f t __T ________ _______ A)/ft' 1. Olisi t oot<4 ________ > Used for MS/D 12 /. o*<,n /. oo%<4 ________ rv/ft a .Ilov 1-011/ /. Oi-ft A OOiZ* f'COWf o-lfi3 < 0 / 8 7 .. Js * J-/Q fi Sts-* Summary of method: Notes: Review Date RU10I39 Form Approved by/Date:_ Form Completioi C SVerified kj 000557 Ion Pair Standard Curvcs-Tissues PrepOale<): I0/I4m Analyst!*): SEE Sample Matrix: Rot Liver Method/Revisioa: ETS-8-6 0 Target Aealyte(s): Fc-Mix Box Number: 0*)-200 Study Number: TOX-145 Equipment Number: 0222-0000 Final Solvent A TN Number: MeOH/TN-A-2945 Blank Tisann/lileutincr Rabbit Liver/99086- 11-5 FC Mix Std Approx. 0 500 ppm: FC Mix Std Approx. 5 00 ppm: FC Mix Std Approx. 50 0 ppm: Surrogate Std Approx. 100 ppm: 09086-47-2 09086-47-1 99095-33 99086-13-11 Actual Concentrations of Standard* m the FC Mix PFOS PFOSA PFOSEA Std Cone Std Conc Std Conc. uit/mL un/mL ug/mL 0 5000 0 5005 0 4997 0 5000 0 5050 0 4997 0 5000 0 5050 0 4997 0 5000 0.3050 0 4997. 0 5000 05050 0 4997 5000 5005 4 997 5000 5 005 4 997 5000 5.005 4997 50 00 50 05 49 97 PFOSAA Std Cone ug/mL 0 4999 0 4999 04999 0 4999 0 4999 4999 4.999 4999 49 99 Blank liver initial density (g) for curves: Final solvent volume (mL) For curves: EtFOSE-OH Std Conc ug/mL 0 500$ 0 500$ 0.500$ 0.5005 0 5005 5X5 SXS 5X5 50 05 MS56 Std Conc. ug/mL 0.S0I0 0S0I0 0 5010 05010 05010 5.010 S.0I0 s.oto 50.10 All Ami Spiked mL 0X2 0004 0010 0 020 0040 0010 0020 0 030 0004 0 163 1 000 AH Density 8 0 163 0 163 0 163 0 163 0 163 0 163 0 163 0.163 0 163 Calculated Concentrations of Standards in the sample matrix PFOS PFOSA PFOSEA PFOSAA Std Conc Std Conc Std Conc. Std Conc. ng/g ng/s ng/g ng/g 6 13 6 14 613 6.13 12.3 124 123 12.3 30 7 3 1 0 307 30 7 61 3 62.0 61 3 61 3 123 124 123 123 307 307 307 307 613 614 613 6)3 920 921 920 920 1227 1228 1226 1227 EtFOSE-OH Std Conc "g/g 6.14 12.3 30 7 6)4 123 307 614 921 1228 M556 Std Conc. ng/g 6.15 12.3 307 61 5 123 307 615 922 1229 Surrogate Std Conc. ug/mL IX Saerogate Final Conc. __ ____ 3077 AB Am i Spiked mL 0.003 Calculated Concentrations of Standards in the 1.0 mL final solvent volume PFOS PFOSA PFOSEA PFOSAA Final Conc Final Conc. Final Conc. Final Cone. ng/mL ng/mL ng/mL ng/mL 100 100 100 l.X 2 .X 2 02 2 0 0 2 .X 5.00 5.05 S X 5 .X 100 10 1 100 10.0 20 0 2 0 2 20 0 200 500 50.1 50 0 500 IX IX IX IX 130 150 150 ISO 200 200 200 2 X EtFOSE-OH Final Conc. ng/mL l.X 2.X SOI 10.0 20.0 50.1 IX ISO 200 M556 Std Conc. ng/mL IX 2.00 SOI 100 200 SOI IX ISO 200 Surrogate Std Conc. ug/mL IX Surrogate Final Conc. ng/mL 502 Afl Am i Spiked mL 0X5 Sample used for MS/MSD 9R03230M. Dyl Control MS/MSD calc. In matrix Initial W t (g): 0 996 PFOS Final Conc. PFOSA Final Conc. PFOSEA Final Conc. ng/g ng/g 301 301 301 301 301 301 PFOSAA Final Conc. ng/g 301 301 Initial Volume (mL): 3.00 E tFO SE -O H M SS6 Final Conc. ng/g 301 Std Conc. "g/g 302 301 302 Approx. Std Cone.. 5.00 ug/mL Ami Spiked (mL) Density 0010 0 166 Sample used for MS/MSD 03230M, Dyl Control MS/MSD calc. In solvent PFOS Final Conc PFOSA Final Conc PFOSEA Final Conc. ng/g ng/g ng/g 50 0 SO 1 50 0 50 0 SO 1 50 0 Sample used for MS/MSD: 9R03235M, Dy4. control MS/MSD calc. In matrix Initial Wt it) 1001 PFOS Final Conc PFOSA Final Conc PFOSEA Final Conc y ng/S ng/S 301 301 301 301 301 30! le used for MS/MSD 03235M. Dy4. control /MSD calc In solvent Initial Wt w) 1 X I PFOS PFOSA PFOSEA Final Cone Final Conc Final Conc. nw * "IPS 50 0 50 1 500 50 0 50 1 500 PFOSAA Final Conc. ng/g 50 0 500 PFOSAA Final Conc ns's 301 301 PFOSAA Final Conc "g/g 500 50 0 Initial Volume (mL): 3 00 EtFOSE-OH M5S6 Final Conc Std Conc. ng/g ng/g 50.1 50 1 30.1 $0 1 Approx. Std Conc 5 00 ug/mL Ami Spiked (mL) Final Vol. 0010 1000 Initial Volume (mL): 3 00 EtFOSE-OH M5S6 Final Conc. Std Conc. ng/g ng/g 301 302 301 302 Approx. Std Cone. 5 00 ug/mL Ami Spiked (mL) Density 0010 0 167 Initial Volume (mL): 5 00 EtFOSE-OH M396 Final Conc. Std Conc ng/g ng/g 50 ! 50 1 $0 1 50 1 Approx. Std Cone. 5 00 ug/mL Ami Spiked (mL) Final Vol 0010 I000 rto d rt t AU Vol. mL 1000 1 000 1000 1 OX 1000 - 1.000 1000 1.000 1.000 Ion Pair Std Extractton Sheet lo-iM-1 * VrvK*d 000558 DILUTIONS SUMMARY SHEET Study: TOX-045 i ,r lqa Dilution Date/Analyst: M CH 10/18/99 MjMr lOjlf Box#: 99-200 sample number or descrpition 1:100 1: 1: 1: 9R03237M, Day 4, Control a UiM- 9R032$5M. Day 1,5 mg/kg 9R03246M. Day 1, 5 mg/kg 9R03247M, Day 1,5 mg/kg 9R03248M, Day 1, 5 mg/kg 9R03249M, Day 1, 5 mg/kg 9R0325IM. Day 4, 5 mg/kg 9R03252M, Day 4, 5 mg/kg 9R03253M, Day 4, 5 mg/kg 9R03254M. Day 4, 5 mg/kg D100 D100 D100 D100 D100 D I00 D I00 D I00 D100 D I00 / Solvent/TN Number: J l^ O H I V ' h ' AAAMt0!^ Extraction Date/Analyst: SEE, 10/13/99 M atrix/Timepoint: Rat Liver DILUTIONS 1: 1: 1: _ Comments Verified By M cm ^ y A tm r ill r1fa ?#-----f--o*/rv / L14- 10[1 tolflr 1 / / J _^ / )1hir{1tw* CC559 Notes: D100=10 uL sample + 990 uL MeOH.IjJJAr lOjlCJ*^ Form Completion Verified Bv: l o - i M ^ j t r Extraction Worksheet ETS-8-4.1 S tu d y # T?-,x- H r M atrix'S, rxt W u rv . Box# 9 9 -jt..o W K /D av I'M D a te S p ik e d /A n a ly s t R B S 1 0 1 9 9 -2 5 0 p p B -C C V -1 1-1 to 4 RTS 10199-250ppb-M S/D -11 RTS 10199-Serum Blank-11412 R B S 10199-H 2O blk-11&12 R B S10199-Serum blk-11&12 R B S 1 0 1 9 9 -5 p p b -1 1 & 1 2 R B S10199-10ppb-11&12 R B S10199-25ppb-11&12 R B S 1 0 1 9 9 -5 0 p p b -1 1 & 1 2 RB S10199-100ppb-11& 12 R B S10199-250ppb-11&12 RB S10199-500ppb-11& 12 RB S10199-750ppb-11& 12 R B S10199-1000ppb-11&12 9R 03230M ,D y1 .Control 9R 0 3 2 3 1 M ,D y 1 , Control 9R 0 3 2 3 2 M ,D y 1 , Control 9 R 0 3 2 3 3 M ,D y 1 , Control 9 R 0 3 2 3 4 M ,D y 1 , Control 9 R 0 3 2 4 5 M ,Dy 1, 5mg/kg 9R 03246M ,D y1,5m g/kg 9R 03247M ,D y1,5m g/kg 9R 03248M ,D y1,5m g/kg 9R 03249M ,D y1,5m g/kg 9R 03235M ,D y4,C ontrol 9R 03236M ,D y4,C ontrol 9 R 0 3 2 3 7 M , Dy4, Control 9 R 0 3 2 3 8 M , Dy4, Coolrol Surrogate Std Approx, ppm Actual ppm #990-4, - 1 1 1 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 ul 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL FC Mix FC Mix FC Mix Com m ents Verified By approx.0.5 ppm approx.5 ppm approx.50 ppm actual ppm actual ppm actual ppm # 99c it, V # W c lC ,T) | # 9 9 0 3 3 lu -H - io - i " - s '!S^r - - 5 L 5 uL aiIA___ l --- --- --- 10 uL - - 20 uL - - - 5 uL - - 10 uL - - 20 uL - - - 5 uL - - 10 uL - - 15 uL - - 20 uL --- -- - - >/ - - - ____ I0w lq ---_- fW A 1 \ ______ --- --- - ----- ! i --- --- --- --- B lan kltabt.;! -fc N Std# q q o o s - 3 l Serum Extraction Method ETS-8-4.1 amount = t -O ml Vortex 15 Sec. P ipette M atrix, spike with ap prop riate su rrog ate or F C -M ix V o lu m e _____ o ml P ip e tte 1 ml o f 0 .5 M T B A , pH 10. o H = i o - 1 0 /1 4 /4 * ? ______ Std. # 4 ^ 0 7 0 - ; v n P ip e tte 2 ml o f 0 .2 5 M N a 2C O j/0 .2 5 M N a H C 0 3 buffer Std. # 9Ctovu> - N - ^ Dispense 5 ml of methyl-t-butyl ether TN-A- bOW u Date & initials l o - t - 9 *>/ 1 /. 1 JIM.lOlMiZ [_______ S hake 20 min C entrifuge 2 0 -2 5 min. R em ove a 4 ml aliquat of organic layer Put on Nitrogen E vaporator to dryness Shaker speed: 3 0 0 Centrifuge speed: 3 V D i J Temperature: Room Temo. m !* imwaism Add m ethanol Vortex 30 sec. Volum e \ O TN -A -^V yV - irnioim'i | Filter using a 3 c c B -D syringe with a 0 .2 um filter into an a u to s am p ler vial u L- (E>> io 9 * ' S--' TK>- r a i aAfy\> n -i o > r v b u \ r W "K"n 990l>lj?? lo-i 10/12/99 Draft Attachm ent A E T S -8 -4 .1 Extraction of P F O S from Serum Form Com pletion , t Verified By MM IfJjptf 000560 Extraction Worksheet ETS-8-4.1 S tU dV #Ti2X W S' M atrix 'kai S -ru -w , Box # W K /D av / ` V D a te 'S p ik e d /A n a ly s t 9R 03239M ,D y4,C ontrol 9R 03250M ,D y4,5m g/kg 9R 03251 M ,D y4,5m g/kg 9R 03252M ,D y4,5m g/kg 9 R 0 3 2 5 3 M ,D y 4 ,5 m g /k g 9 R 0 3 2 5 4 M ,D y 4 ,5 m g /k g -- - - - - - - - - - - - - - y yy U - .................................... S urro gate Std Approx, ppm Actual ppm nWon.isi i IOiO 5uL 5 uL 5 uL 5 uL 5 uL 5 uL - y y y FC Mix FC Mix FC Mix approx.0.5 ppm approx.5 ppm approx.50 ppm actual ppm actual ppm actual # ,j A # iA (V ^ # rt ppm - --- - --- --- -- - ------------- ---------- 7 - - - - - -y y -yiy yyy' - - y - - / -/ y y - K -- -- - --- -- - - . ---- - Com m ents Verified By rt- hjl rt __ --- - --- - --- - --- - --- - - /- - - -- -- -- --------- - =" ' > Vortex 15 Sec. Pipette M atrix, spike with appropriate surrogate or FC -M ix V olum e / O Pipette 1 ml of 0.5 M TBA, pH 10. p H = ia . P ip e tte 2 ml o f 0 .2 5 M N a 2C O j/0 .2 5 M N a H C Q 3 bu ffer Std. # . Dispense 5 ml of methyl-t-butyl ether T N -A -, S h ak e 2 0 min Centrifuge 2 0 -2 5 min. _Cen^fege_s^ed^^^^ Remove^a^^mlaiiquatof^rganiclayer^ Put on Nitrogen Evaporator to dryness Tem perature: RoomlfiSET Add m ethanol V o lu m e , i_i2_ TN-A-^ Vortex 30 sec. Filter using a 3c c B-D syringe w ith a 0 .2 urn filter into an autosam pler vial Cont. Cal. Verifications used sam e m atrix as for std curve. ml Date & Initials JO: /-*>/- <y 10/12/99 Draft Attachm ent A E T S -8 -4 .1 Extraction of P FO S from Serum Form Com pletion , / Verified ByJillrl l)j)^ 000561 Sample Weights/ Volumes Prep Date(s): 10/19/99 Analyst^): SEE Sim ple Matrix: Rat Serum Method/Revision: ETS-8-4 I Target Analyte(s): PFOS, PFOSA Sample ID 9R03230M,Dy 1,Control 9R03231M,Dyl,Control 9R03232M,Dyl .Control 9R03233M,Dyl,Control 9R03234M,Dyl .Control 9R03245M,Dy 1,5mg/kg 9R03246M,Dy 1,5mg/kg 9R03247M,Dyl,5mg/kg 9R03248M,Dy 1,5mg/kg 9R03249M,Dy 1,5mg/kg 9R03235M,Dy4,Control 9R03236M,Dy4,Control 9R03 237M,Dy4,Control 9R03238M,Dy4,Control 9R03239M,Dy4,Control 9R03250M,Dy4,5mg/kg 9R03 251 M,Dy4,5mg/kg 9R03252M,Dy4,5mg/kg 9R03 254-1 M,Dy4,5mg/kg 9R03254-2M,Dy4,5mg/kg Initial Voi. mL __ I- 0 OnL______ Study Number: TOX-145 Box: 99-206 Final Solvent & TN Number: MeOH/TN-A-2945 Matrix Blank/Identiner: Rabbit Serum/99062-39 Rat Serum/99062-88 Verified By: Comments w /# L______ -- 1 i --- - - Summary of method: -- :zzj . n ---- w S O - ' Notes: Review Date &lf>Rtsl0199 000562 Ion Pair Standard Curvea-Fluidi Prrp >*<): A aalyit(a): Sample Matrix: Method/Revitiea: Target Aalyle<i): Bex Number: 10/14/09 SEE Rat Serum ETS-8-4 I PFOS. PFOSA 09.206 Study Number: TOX-I4S Egeipmcet Number: Pinal Salvent * TN Number: MeOH<TN-A'2945 Bleak TiMne/ldentifler: Rabbit Senm/90062-}9 Rat Scrum/99062-SS FC Mi Std Approx. 0 500 ppm: PC Mix Sid Approx. 5 00 ppm: FC Mix Std Approx. SO0 ppm: SurfOfate Std Approx. 100 ppm: 99086-47-2 99086-47-1 99095-3} 99086-13-11 Actual Concemmtofl o f Standards in the FC Mix PFOS PFOSA PFOSEA Std Cone. Std Cone. Std Cone ug/mL utt/mL ug/mL 0 5000 0 5005 0 4997 0 5000 0 5005 04997 5.000 5 005 4997 3 000 5 005 4 997 5000 5 005 4 997 50.00 5005 49 97 50 00 50 05 49 97 50 00 50 05 49 97 50 00 SO05 49 97 PFOSAA Std Cone. ug/mL 0 4999 0 4999 4.999 4.999 4 999 49 99 49 99 49 99 49 99 EtFOSE-OH Std Cone. ug/mL 0 5005 0 5005 S 005 5.005 5.005 $0 05 SOOS 50 05 50 05 Blank mrum initial volume (mL) or narres: Final aolvent volume <mL) fur enrvea: I 00 100 MSS Std Cone. ug/mL 05010 osoto 5010 5010 $.010 50.10 50.10 50 10 50 10 All Amt Spiked mL 0.010 0.020 0.003 0.010 0.020 0.003 0010 0.015 0.020 All nidal Votum mL 1.015 1.025 1.010 1 0IS 1.025 1.010 1.015 1.020 1.025 All Final Vol. mL 100 1 00 1 00 100 1.00 1 00 1.00 1.00 1 00 Calculated Concentrations o f Standard ia the ampio matrix PFOS PFOSA PFOSEA Std Cone. Std Cone. Std Cone. fiK/mL 493 ng/mL 493 ng/mL 4 92 9 76 9.77 9 75 24.8 24 8 24 7 49.3 49 3 49 2 97.6 97.7 975 248 248 247 493 493 492 735 736 735 976 977 975 PFOSAA Std Cone. ng/mL 493 9.75 24.7 49.3 97.5 247 493 735 975 EtFOSE-OH " Sul Cone. ng/mL 493 9 77 24.8 49 3 97 7 2a 493 736 977 MSS Std Cone. ng/mL 494 971 24.8 494 97.1 248 494 737 978 Surrogate Std Cone. ugtoiL 101 Surrogate Final Cone. ng/mL 496 AM Amt Spiked mL 0 005 Calculated Concentrations o f Standard a the 1.0 mL final solvent volume PPOS PFOSA PFOSEA PFOSAA Final Cone. ng/mL 5 00 Final Cone. ng/mL 501 Final Cone. ng/mL 5 00 Final Cone. ng/mL 5 00 10.0 100 100 100 25.0 25.0 25.0 25.0 50 0 50.1 $00 500 100 100 100 100 250 250 250 250 500 501 500 500 750 751 750 750 1000 1001 999 1000 EtFOSE-OH Final Cone. ng/mL 501 10.0 25.0 50.1 too 250 SOI 751 1001 MSS Std Cone. ng/mL SOI 100 25 1 50 1 100 251 SOI 752 1002 Surrogate Std Cone. ug/mL 101 Surrogate Final Cone. ng/mL 503 ----- AB Amt Spiked mL 0 005 Sample used for MS/MSD: Rat control tsun99062-U MS/MSD Cone, in the ample matrix PFOS PFOSA PFOSEA Final Cone. Final Cone. Final Cooc. ng/mL ng/mL ng/mL 248 248 247 248 248 247 Sample used for MS/MSD: Rat control *en*iv99062-88 MS/MSD Cone, in the final solvent PFOS PFOSA PFOSEA Std Cone. Std Cone. Std Cone. ug/mL ug/mL ug/mL 250 250 250 250 250 250 Initial Volume (aiL): 1.00 PFOSAA EtFOSE-OH MSS Final Cone. Final Cone. Std Cone. ng/mL 247 247 aitaL 2a 2a (M . 2a 248 Approx. Sid Cone.: 50.0 ug/mL Amt Spiked Vol. (mL) 0005 Initial Volume (mL): 1.00 PFOSAA EtFOSE-OH MSS Std Cone Sid Cone Sid Cone. ug/mL ug/mL ug/mL 250 250 251 250 250 251 Approx. Std Cone.: 50.0 ug/mL Amt Spiked Vol. (mL) A* 0 005 Cud Final Vol. (mL) 1 00 All TV. n\ul \fi( \tj, RUI0I99 Form Completion Verified 000563 DILUTIONS SUMMARY SHEET Study: TO X-145 Dilution Date/Analyst: M C H , 10/21/99 Box#: 99-206 .. M '' sam ple num ber or descrpition 1:50 9R03245M, Day l,5mg/kg D50 9R03246M, Day i, 5mg/kg D50 9R03247M. Day 1,5mg/kg D50 9R03248M, Day l,5mg/kg D50 9R03249M, Day l,5mg/kg D50 9R03250M, Day 4, 5mg/kg D50 9R03251M, Day 4, 5mg/kg D50 9R03252M, Day 4, 5mg/kg D50 9R03254-1M, Day 4, 5mg/kg D50 9R03254-2M, Day 4, 5mg/kg D50 1: - 1: . _ . . 1: . . _ 1: . . . . . _ - Solvent/TN Number: M eO H , TN-A-2945 Extraction Date/Analyst: SEE, 10/19/99 M atrix/Tim epoint: R at Sera Days 1&4 DILUTIONS I: i: . ._ __ ._ .. __ .. _ _. Comments M//V / / i/ Verified By /M n AJ//V / f 000S64 ( 'v_______ _________ ____ Notes: D50=20 uL simple + 980 uL MeOH. Form Completion Verified Bv: <&*tC Extraction Worksheet ETS-8-6.0 S tu d v# 7 V /y-> Matrix Box# ik*'*-A ' I f 7 / , ` - p o i , _____________ W K /D av / / A ftriL D a te S p ik e d /A n a ly s t -H 20 B lk - / -LiverBIk - 1 -6ppt>-1 -12ppb-1 -30ppb-1 -60ppb-1 -120ppb-1 -300ppb-1 -600ppb-1 ! -900ppb-1 4/ -1200ppb-1 Surrogate Std Approx ppm A ctu al lei p p m ic/l 1J99~ J tW 5 . 0 ul 5 . 0 ul 5 . 0 ul 5 . 0 ul 5 . 0 ul 5 . 0 ul 5 . 0 ul 5 . 0 ul 5 . 0 ul 5 . 0 ul 5 . 0 ul F C Mix F C Mix FC Mix I C om m ents I Verified By 1 approx.0.5 p p m approx.5 p p m approx.5 0 ppm actual # ppm actual p p m actual Mf t f c 1\/ 7 - # ppm -W ) / h * w (? ^ ' 2 ul / / / / / rr 1 4 ul 1 0 ul (p / " / / rr1 ri 2 0 ul 4 0 ul y y / y y r 1 0 ul 2 0 ul 3 0 ul / / / 4 ul I _____ 1n n I__________ \ --- \ \ V - __ * i i I ! ,, ----------- 1 / 7 / 7 A / 9 - 9 I -------------------- -- I ------- ------- ^ -- --------" .. i I Blank - rhkhih __ std# 9?oi~ / / - Liver Extraction Method__ ETs-8-6.0 r = /a m o u n t > ml -- __ -- ./3 g/m l Data & Initials -- -- " j_=* hk Vortex 15 Sec. P ipette M atrix, spike with appropriate s u r r o g a t e o r FC -M ix P ipette 1 ml o f 0 .5 M TB A , dH 10. dH= fa !oMt9 Volume Std ____ r*/w -ft (, 0 ml # JJ4Z=1& _____I P ipette 2 ml o f .23 M N a ,C 0 V 0 .^ 5 M N a H - b u f f e r D ispense 5 ml o f methyl-t-butyl ether std.# t n -a - P-Mc, ss "j S h ak e 2 0 min Centrifuge 2 0 -2 5 min. S h a k e r sp eed :_ C e n t r i f u g e speed: _ f /? I ! |R em ove a 4 ml aliquat of organic layer Put on Nitrogen Evaporator to dryness |Add methanol Volum e i i ml Ie m p e r ature: R o o m te m o . 9 9 ST N - A - | ..-- -- 1 s 1 IVortex 30 sec. a| F ilte r using 3 c c B -D syrin g e w ith a 0 2 u r n filter i n t o a n a u t o s a m p l e r v i a l Cont. Cal. Verifications used same m a t r i x a s f o r s t d c u r v e . || 7/ Z Z 10/12/99 Draft Attachment A ETS-8-5 0 ofE x t r a c t i o n P F O S f r o m Liver Form Completion Verified IPfarfU 000565 lofi Pair Standard Curves-Tissues Prep Dateti): Anaiyst(s): Sim p le Matrix: M e lh od /R evisio n : Target Analyte<s): Bai Number: 10/25/09 RWW /V u /lv Rabbit Liver ETS-8-6.0 See below 99-206 FC Mix Sid Approx. 0.500 ppm: FC Mix Std Approx. 5.00 ppm: FC Mix Std Approx. 50.0 ppm: Surrogate Std Approx. 101 ppm: 99086*44*3 99086-44-2 99086-44-1 99086-13-11 Actual Concentrations o f Standards in the FC Mix PFOS PFOSA EtFOSE-OH Std Cone. Std Cone. Std Cone. ug/mL ug/mL ug/reL 0.5004 0.3000 0.5000 0.5004 0.5000 0.5000 0.5004 05000 0.5000 0.5004 0.5000 0.5000 0.5004 0.5000 0.5000 5.004 5.000 5.000 5.004 5 000 5.000 5.004 5.000 5.000 50.04 50.00 50.00 MSS6 Std Cone. ug/mL 0.5000 0.5000 0.5000 0.5000 0.5000 5.000 5.000 5.000 $0.00 Calculated Concentrations o f Standards to the sample matrix PFOS PFOSA EtFOSE-OH M556 Std Cone. Std Cone, Std Cooc. Std Cone. ng/g ng/g n t/t 8/8 6.14 6.13 6.13 6.13 12.3 12.3 12.3 12.3 30.7 30.7 30.7 30.7 61.4 61.3 61.3 61.3 123 123 123 123 307 307 307 307 614 613 613 613 921 920 920 920 1228 1227 1227 1227 Study Number: TOX145 Equipment Number: Final Solvent Jk TN Number: MeOH/TN-A-2945 Rabbit Liver/99086-13-5 M570 Std Cone. ug/mL 0.5000 0.5000 0.5000 0.5000 0.5000 3.000 5.000 5.000 50.00 M570 Std Com . ng/g 6.13 12.3 30.7 613 123 307 613 920 1227 Blank liver inilial density (g) for curves: Final solvent volume (mL) for curves: 0.163 1.000 McFOSE-OH Std Cone. ug/mL 0.5000 0.5000 0.5000 0.5000 0.5000 5.000 5.000 5.000 50.00 POAA Std Cone. ug/mL 0.5000 0.5000 0.5000 0.5000 0.5000 5.000 5.000 5.000 50.00 PFHS Std Cone. ug/mL 0.5000 0.5000 0 5000 05000 0.5000 5.000 5.000 5.000 50.00 All Am't Spiked mL 0.002 0.004 0.010 0.020 0.040 0.010 0.020 0.030 0.004 All Density 8 0.163 0.163 0.163 0.163 0.163 0.163 0.163 0.163 0.163 AU Vol. mL 1.000 1.000 1.000 1000 1.000 1.000 1.000 1.000 1.000 MeFOSE-OH Std Cone, ng/g 6.13 12.3 30.7 61.3 123 307 613 920 1227 POAA Std Cone, ng/g 6.13 12.3 30.7 61.3 123 307 613 920 1227 PFHS Std Cone, ng/g 6.13 12.3 30.7 61.3 123 307 613 920 1227 Surrogate Std Cone. ug/mL 101 Surrogate Final Cone. ng/g 3098 All Am't Spiked ml. 0.005 ___ Calculated Concentrations o f Standards in the 1.0 mL final solvent volume PFOS PFOSA EtFOSE-OH M5S6 Final Cone. Final Cooc. Final Cooc. Final Cone. ng/raL ng/mL ng/mL ng/mL 1.00 1.00 1.00 1.00 2.00 2.00 2.00 2 00 5.00 5.00 5 0 0 5.00 10.0 10.0 10.0 10.0 20.0 20.0 20.0 20.0 50.0 50.0 50.0 50.0 100 100 100 too 150 150 150 150 200 200 200 200 M570 Final Cooc. ng/mL 1.00 200 5.00 10.0 20.0 50.0 100 150 200 MeFOSE-OH Std Cone. ng/mL 1.00 2.00 5.00 10.0 20.0 50.0 100 150 200 POAA Std Cooc. ng/mL 1.00 2.00 500 10.0 20.0 50.0 100 150 200 PFHS Std Cone. ng/mL 1.00 2.00 5.00 10.0 20.0 50.0 100 130 200 Surrogate Std Cooc. ug/mL 101 Surrogate Final Cone. ng/mL 505 All Am't Spiked ml. 0.005 Sample used for MS/MSD: MS/MSD cak. In matrix PFOS Final Cooc. ng/g 300 300 No MS/MSD Initial W t (g): 1000 PFOSA EtFOSE-OH Final Cone. Final Cone. ng/g ng/g 300 300 300 300 MS56 Final Cone. ng/g 300 300 Initial Volume (mL): 5.00 M570 MeFOSE-OH Final Cooc. Std Cone. ng/g ng/g 300 300 300 300 Sample used for MS/MSD: MS/MSD calc. In solvent PFOS Final Cone. ng/g 50 50 No MS/MSD PFOSA Final Cone. ng/g 50 50 E lF O S E ^ H Final Cooc. ng/g 50 50 M556 Final Cone ng/g 50 50 Initial Volume (mL): 5.00 M570 MeFOSE-OH Final Cooc. Std Cone. ng/g ng/g 50 50 50 50 POAA Std Cooc. ng/g 300 300 POAA Std Cone. ng/g SO 50 Approx. Std Cone,: 5.00 ug/mL Ain't Spiked (mL) PFHS 0.010 Std Cone. ng/g 300 300 Density 0.167 Approx. Std Cone.: 5.00 ug/mL Am't Spiked (mL) PFHS 0.010 Std Cone. ng/g 50 50 n j l n t l Final Voi. 1.000 lPSE-10259Liv-99086-44-l \ts l on r h i C C aG 6 Extraction Worksheet ETS-8-4.1 Study # S u r r o g a t e Std M atrix y?j / / J>f '* * A pprox p p m B o x # 99 Actual ppm W K/Day O a te S p ik e d /A n a ly s t CfiSisnt -H 2 0 B lk - > # hkJ*4h&Vv 5 . 0 ui -SeraBIk _ / 5 . 0 ul -5ppb --/ -10ppb - 1 5 . 0 ul 5 . 0 ul -2 5 p p b '/ - 5 0 p p b _ 5 . 0 ul 5 . 0 ul / -100ppb- / 1 -250ppb_ 1 5 . 0 ul 5 . 0 ul -500ppb - / 5 . 0 ul -750ppb - / 5 . 0 ul -1000ppb - / 5 . 0 ul ---------------- ^^ F C Mix F C Mix FC Mix Com m ents approx.0.5 p p m approx.5 p p m approx.50 ppm actual ppm actual p p m actual ppm 9fefc -W - J # 9?e*c-W-f i totr\ /t/uU* ______ t O ifl_____ 0 a ______l ! \ I 1 0 ul | 2 0 ul A) J______ % 5 ul 1 0 ul _______L _ 2 0 ul if | 5 ul I 10 ul * t_______ t 1 5 ul 2 0 ul ............j Verified By 1 L = t= J/ / i /< v ^ < I i i I i _<__ .____ ___ -- Blank /h U -t i / s y S t d # T/9-A - 1 i X i . S e r u m E x tra c tio n Method E T S -8 -4 .1 Vortex 15 Sec. P ipette Matrix, spike w ith appropriate s u r r o g a t e o r F C - M i x Pipette ml of 0 .5 M TB A , pH 10. p H = /^ lP ip e tte m l o f 0 .2 5 M N a 2C 0 3 /0 .2 5 M N a H C C A b u f f e r D ispense 5 ml of methyl-t-butyi ether U 0 .a m o u n t = ml D ate & In itials /o/!hJ> * ~ Volume i,o ml S t d . # 9<r>Z6 SJ-t< S t d . # 9eoTt-M-QV T N -A - J-99C A L ........ 1" S h a k e 2 0 min Centrifuge 2 0 -2 5 min. S h a k e r speed: _3C e n t r l f u q e s p eed : &O R em ove a 4 ml aliquat of organic layer Put on Nitrogen Evaporator to dryness Add m ethanol Volum e ft n Temperature: I TN-A- R o o m IemD. ^ 9<f f Vortex 30 sec. Filter using a 3 c c B -D syringe with a 0 . 2 u m filter i n t o a n a u t o s a m p l e r v i a l Cont. Cal. Verifications used same m a t r i x a s f o r s t d c u r v e . to lL i'h 9 -//> j J/ . -- "> 10/12/99 Draft Attachment A ETS-3-4 ofa c t i o n PFOS 1 troni S e r u m Form Completion Verified By ic 000537 Ion Pair Standard Curvcs-Fluidi Prep Dated): Analysed): Sample Matrix: M e tbod /R evisio n : Target Analyted): Bex Number: 10/25/99 RWW f t Rabbit Serum ETS-S-4.1 Below 99-206 FC Mix Std Approx. 0.500 ppm: FC Mix Std Approx. 5.00 ppm: FC Mix Sid Approx. 50.0 ppm: Surrogate Std Approx. 101 ppm: 99086-44-3 99086-44-2 99086-44-1 99086-15-11 Actual Concentrations o f Standards ia the FC Mix PFOS PFOSA EtFOSEOH Std Cone. Std Cone. Std Cone. ug/mL ug/mL ug/mL 0 5000 0.5000 0.5000 0 5000 05000 0.5000 05000 0.5000 0.5000 5.000 5 000 5 000 5.000 5.000 5.000 5.000 5.000 5.000 50.00 50 00 50 00 50.00 50.00 50 00 50.00 50.00 50.00 30.00 50.00 50.00 MS56 Std Cone. ug/mL 0.5000 0.5000 0.5000 $.000 5.000 3.000 50.00 50.00 50.00 50, Off Calculated Concentrations o f Standards in the sample matrix PFOS PFOSA EtFOSEOH Std Cone. Std Cooc Std Cone. ng/mL ng/mL ng/mL VALUE! VALUE! VALUE! 4,93 4.93 4.93 9.76 9.76 9.76 24.8 24.8 2 4 8 49.3 49.3 49.3 97.6 97.6 97.6 248 248 248 493 493 493 735 735 735 976 976 976 MS56 Std Cone. ng/mL VALUE! 4.93 9.76 24.8 49.3 97.6 248 493 735 976 Study Number: TOXI43 Equipment Number: Final Solvent k TN Number: MeOII/TN-A-2945 Blank TUsue/ldcntiflcr: Rabbit Sera/TNA-2382 MS70 Std Cone. ug/mL 05000 05000 05000 5.000 5.000 5.000 50.00 50.00 50.00 50.00 MeFOSCOH Std Cone. ug/mL 0.5000 0.5000 0.5000 5.000 5.000 5.000 50.00 30.00 50.00 50.00 Blank scrum initial volume <mL) for curves; Final solvent volume (mL) for curves: l .00 1.00 POAA Std Cone. ug/mL 0 5000 0.5000 0 5000 5.000 5.000 5.000 50.00 50.00 50.00 50.00 PFHS Std Cone. ug/mL 0.5000 0.5000 0.5000 5 000 5.000 3.000 50.00 50.00 50.00 50.00 All Am't Spiked mL 0.010 0.020 0.005 0.010 0.020 0.005 0.010 0.015 0.020 All Initial Volume mL VALUE! 1.015 1.025 1.010 1.015 1.025 1.010 1.015 1.020 1.025 All Final Vol. mL 1000 1.000 1.000 1.000 1.000 1.000 1.000 1.000 1.000 1.000 MS70 Std Cone. ng/mL VALUE! 4.93 9.76 24.8 49.3 97.6 248 493 735 976 MeFOSEOH Std Cone. ng/mL 1 VALUE! 4.93 9.76 24.8 49.3 97.6 248 493 735 976 POAA Std Cooc. ng/mL VALUE! 4.93 9.76 24.8 49.3 97.6 248 493 735 976 PFHS Std Cone. ng/mL VALUE! 4.93 9.76 24.8 49.3 97.6 248 493 735 976 Surrogate Std Cooc. ug/mL 101 Surrogate Final Cone. ng/mL 498 -- All Am't Spiked mL 0.005 Calculated Cooccndadons o f Standards in the 1.0 mL final solvent volume PFOS PFOSA EtFOSEOH M556 Final Caie. Final Cooc. Fumi Cooc. Final Cone. ng/mL ng/mL ng/mL ng/mL VALUE! VALUE! VALUE! VALUE! 5.00 5 00 5.00 5.00 10.0 100 10.0 10.0 25.0 25.0 25.0 25.0 50.0 5 0 0 50.0 50.0 100 100 100 100 250 250 250 250 500 500 500 500 750 750 750 750 1000 1000 1000 1000 M570 Final Cooc. ng/mL VALUE! 5.00 10.0 25.0 50.0 100 250 500 750 1000 MeFOSEOH Std Cone. ng/mL VALUE! 5.00 100 25.0 50.0 100 230 500 750 1000 POAA Std Cone. ng/mL VALUE! 5.00 10.0 25.0 50.0 100 250 500 750 1000 PFHS Std Cooc. ng/mL VALUE! 5.00 10.0 23.0 50.0 100 250 500 750 1000 Surrogate Std Cooc. ug/mL 101 Surrogate Final Cone. ng/mL 505 All Am't Spiked m l. 0.005 Sample used for MS/MSD: NoM S/M SD MS/MSD Cone, in the sample matrix PFOS PFOSA Final Cone. Final Cooc. ng/mL ng/mL 248 248 248 248 Sample used for MS/MSD: No MS/MSD MS/MSD Cone, in the final solvent PFOS PFOSA Std Cone. Std Cooc. ug/mL ug/mL 250 250 250 250 EtFOSEOH Final Cooc. ng/mL 248 248 EtFOSEOH Std Cooc. ug/mL 250 250 Approx. Std Cone.: 50 ug/ml Initial Volume (mL): 1.00___________ 2,00______________________________ M556 M570 MeFOSEOH POAA PFHS Final Cone. Final Cone. Std Cone. Std Cone. Std Cone. ng/mL ng/mL ng/mL ng/mL ng/mL 248 248 248 248 248 248 248 248 248 248 Initial Volume (mL): 1.00___________ 2.00 MSS6 MS70 MeFOSEOH POAA Std Cone. Std Cone. Std Cone. Std Cone. ug/ml 250 ug/mL 250 u g/m l 230 ugmL 250 250 250 250 250 Approx. Std Cone.: SOug/ml PFHS Std Cone. ug/mL 250 230 Ain't Spiked Vol. (mL) Am t Spiked Vol (mL) 0005 Final Vol. (mL) IPSE- !0259Ser-99086-44- ! xls /o /j r /t f 000568 Prep Dateli): Analyitli): J 5 |* Sample M atrix: ~Juk*.h. &> Mcthod/Revision: Target Analyte(s): f f e s / p b A ^ Sample Extraction Sheet Study Number: T fi& t/yg' Equipment Number: Notebook# and Page: Final Solvent: f(* H 7 ^ - A ^ i T - Procedure Detail ^**7A-4- jLSa_AceA**. a.<J ZmA 7 ; i; tem Ji/ m*. /7_Pf*/ S Jo**., h***-/' JJ*-___________ _________T__O__ & J & L . ...... ____ _____________________________ ****rt>T___ to/la(di*j dt/iJ-ttKi Am** J**4- u *-" l ? 0 A * (7 F + s - I t o s i - * J - ? * * * * * :* > - * tP * A o FF*? .* I ' / r____________________________________________________________________ _________1 ___________ 3*-n> -- ffogj -i3-tt Jq/ffm. 7P*C /T aA______________________________________________ _______________ ^ ? s * ~ [ L 0 ---------------------------------------------------------------------------------------------- ________ T X a g c x / d o o K fT a t- * - -- Z a f j t l ______________________ U s e ..* * * _______________________________________________ ________ j n ________________________5 ^ * - J f / b o a A - / Q O ......" t - ,>gz ____ / _ ______ _______ E x traction-1 T e m p la te R e v i e w D a t e __________________ E m p o re E x tra c tio n P 3 .x ls Page I o f 0005G 9 Sample Extraction Sheet Prep Dateli) r f * f / t f Analyxt(i): * Sam ple M atrix: <^Tf , ^ t n Vlethotl/Revision: Target AnH lytc(s):^9 //% y^( _____________ES&s___ Study Number: Toxr/s Equipment Number: Notebook# and Page: Final Solvent: Procedure Detail 'TU T*-'*-*F*S' U * 3of A T fc s A * / * . _l__^__L__ . __(_*__- _ . __`/___--_ ___/_t_e__c__/___"__* ____ 2 `A T lU z . * . t f b M . y y * * * * * .(/ M a J y tY i. . * * - i d u r f* / 7 f c s A ^ a * - d ? o > M b * .+ a - f L i r i x n r c ___ t & a A m L - / . / 7 ^ cav. U j & M J > /> T ie ___ t K -f ce .. e / d x e ! ---------------------------------------------------------------------------------------------------------------------------- U ~ tJ - ffc s A ^ tf T L - /* T fV -- t / ' /tQ " * < / > * /a a T fr W ftM * ~ n a n - 3 ^ 3 a to J fT j* . - y T F + v fitA A , 'T in * . : / Q 4 / a o * $ L .C - Z ffl ^ T fr c- *< ^ y -i* ^ + Jagg x Q-/atmL___s , i ^ i r ^^ F .xtra ctio n -I T e m p la te R e v i e w D a t e ____________ EmporeExtractionP3.xls Page I of o o o sv o Prep Dated): t'f a M A nalyild): -*'s Sam ple M atrix: Tkx**^ M ethod/R eviaion: T arg et A n a ly te d ): /-3=o j A _______ Procedura Datait Sample Extraction Sheet Study Numfctr: / x ^ / ^ S Equipment Number: Notebook* and Page Final Solvent: J/V fu i--A - 7 f rf ' A r, ?f c0 t*f AA XZ -x*x.*.**+ oLL. -- &* +L -- ( ft Jn l jK& t yL J -L j i r /( X ' < W a P A h - r / '7 M X - < fo 4 * k i / - o r. k .x_ ____ * c ____ " f r o * * , - t f * \ j - / W m__ U. i ___________y__j-_r^muSk,m______ ^ / m s ___ b * U 1L 3i -/j . . 4. . k .! . . ^a t V /nfefx. - / L t--/ *4 s i p j * c / r r / /x rU -----A L t-- L * / c t < * * , /------ ? - / j //-> Wtarji /(L d te ^ f J f tr t- i t F q sa - T t e /T j a a - - / - P t -3 ? --3 ^ / o / p r t ^ - < < /> d L S j j i ^ -- g 4 -frk Y F q s I T o a a - ______________ Tb^e. ~ ------A C fou^L- s: -MS 3 - * * > t T - . / .j R P f f k X % i/- ... - ------------------------------ ( t>. 2o.>U.'> - __ { i * o 'i / r b A , - \ ttX A Qg<-- ____________________________________________ ^r> M . IJ .Z a x x.L . A f o n o c "oo S M S ,A7f / r /O r * X 0 .2 ja n -t- je /f lo j 2 o a ^ p X __ x Q./ n o t , * *a ./ O xW . tu U . x loop = Joc^L /ar-b- T L ^ r z r 3 x > t> ^ , M S5, & t rr<e *i rfpa. i h i * r - -- 3 p na>yAf f^t.-- Tfojx ~- /A?/-~trr y h2iiLe-A _ - i u d j i t ________4__k__________2__&. J*k ^ : ___V ' ....O m J O Q y f A , U J s . tT " f/./y - L - J /A . /0 * * -L f 4 * J i E t traction-1 Template Rcvkw Otite_________ Extraction eli / /J Form Approved by/Bte:' Paqe I ot' 0005T I Extraction Worksheet ETS-8-4.1 Study # TQX 145 Matrix: Rat Sera Box # 99-2Q8 WK/Dav: Dav 29 DateSpiked/Analyst RBS11039-250ppb-CCV9410 RTS11039-SeraBlk-9410 Fkj-i RTSl1039-250ppb-MS9 RTS11039-250ppb-MSD10 RBS11039-H20Blk-9410 RBS11039-SeraBlk-9410 RBS11039-5ppb-9&10 RBS11039-10ppb-9&10 RBS11039-25ppb-9410 RBSl1039-50ppb-9&10 RBS11039-100ppb-9410 RBS11039-250ppb-9410 RBS11039-500ppb-9410 RBS11039-750ppb-9410 F i J- a RBS11039-1000ppb-9410 9R03240M-0-Day 29 9R03241M-0-Day 29 9R03242M-0-Day 29 9R03243M-0-Day29 9R03244M-0-Day29 9R 0325S M -5m g/kg-O ay 29 9R 03256M -5m g /k g -D ay 29 _ Surrogate Std FC Mix FC Mix FC Mix Comments Approx. 100ppm approx.0.5 ppm approx.5 ppm approx.50 ppm Actuahci ppm actual c.-T ppm actual <~-c ppm actuals*; cppm ^ IR U -Ib -Il 7-a 7-I UttA 11/07/4* 5 uL - hum nfoil w - 5 uL 5 uL - - - 5 uL - - 5 uL 5 uL - - 5 uL 5 uL - - - 5 uL - - - 5 uL 10 uL - - 5 uL 20 uL - - 5 uL - 5 uL - 5 uL - 10 uL - 5 uL - 20 uL - 5 uL - - 5 uL 5 uL - - 10 uL 5 uL - - 15 uL 5 uL - - 20 uL 5 uL - - - 5 uL - - - 5 uL - - - \ 5 uL - - - \ 5 uL - - -\ 5 uL 5 uL -- --- - _______ L _ - Verified By 1 \ ) fI 1 J/A 9R 03257M -5m g /k g -D ay 29 5 uL - - - 9R 03258M -5m g /k g -D ay 29 5 uL 9R 03259M -5m g /k g -D ay 29 5 uL Blank: Rabbit Sera S td # q%\j a - 9 * Serum Extraction Method ETS-8-4J. - amount * 1 . 0 ml -j - _______ Sst Date & Initials Vortex 15 Sec. Filter using a 3cc B -D syringe with a 0 ,2 um filter into an au to s am pler vial Cont. Cal. Verifications used sam e matrix as for std curve. F N -1 : T h e M S /M S D and associated sera blanks w ere taken from control rat sera T C R ^ C w ^ '*? C . FM -J U0 i \ - '.C oC ^\o " `I j_ ''C.t'iCc' A f t e v O cW y -* X ? _ F , y b a c u iy\clF TkCl\ iO-vnpi-C. OoF <.o iv y le f f O .A C V f . , s W < r <a ^ - r - x SK e t w c A a is , 111 C i | 10/12/99 Draft Attachm ent A E T S -8 -4 .1 Extraction of P F O S from Serum Form Completion Verified By Jco 000572 0 Ion Pair Standard Curvcs*-Semm PrvpDalets): 11/03/99 Analyses): MCH Sample Matrix: Rat Sera Mefhod/Revision: ETS-8-4 I Target Analyte(s): PFOS. PFOSA Bex Number: 99-208 FC Mix Std Approx. 0.500 ppm: 99086-47-2 FC Mix Std Approx. 5.00 ppm: 99086-47-1 FC Mix Std Approx. 50.0 ppm: 99095-33 Surrogate Std Approx. 100 ppm: 99086-13-11 Actual Concentrations of Standards in the FC Mix PFOS PFOSA PFOSAA Std Cone. Std Cone. Std Cone. ug/mL ug/mL ug/mL 0.5000 0.5005 0.4997 0.5000 0.5005 0.4997 5.000 5.005 4.997 5.000 5.005 4.997 5.000 5.005 4.997 50.00 50.05 49.97 50.00 50.05 49.97 50.00 50.05 49.97 50.00 50.05 49.97 EtFOSE Std Cone. ug/mL 0.4999 0.4999 4.999 4.999 4.999 49.99 _ 49.99 49.99 49.99 Calculated Concentrations of Standards in the sample matrix PFOS PFOSA PFOSAA Std Cone. Std Cone. Std Cone. ng/mL ng/mL ng/mL 4.93 4.93 4.92 9.76 9.77 9.75 24.8 24.8 24.7 49.3 493 49.2 97.6 97.7 97.5 248 248 247 493 493 492 735 736 735 976 977 975 EtFOSE Std Cone. ng/mL 4.93 9.75 24.7 49.3 97.5 247 493 735 975 Study Number: TOXI45 Equipment Number: Final Solvent & TN Number: MeOH TN-A-2997 Blank Tissue/Identifier: Rabbit Sera TCR99062-94 PFOSEA Std Cone. ug/mL O.SOOS 0.5005 5.005 5.005 5.005 50.05 50.05 50.05 50.05 Blank serum initial volume (mL) for curves: Final solvent volume (mL) for curves: 1.00 1.00 M556 Std Cone. ug/mL 0.5010 0.5010 5.010 5.010 5.010 50.10 50.10 50.10 50.10 All Ami Spiked mL 0.010 0.020 0.005 0.010 0.020 0.005 0.010 0.015 0.020 AU Initiai Volum mL 1.015 1.025 1.010 1.015 1.025 I.OIO 1.015 1.020 1.025 AU Final Vol mL 1.000 1.000 1.000 1.000 1.000 1.000 1.000 1.000 1.000 PFOSEA Std Cone. ng/mL 4.93 9.77 24.8 49.3 97.7 248 493 736 977 MS56 Std Cone. ng/mL 4.94 9.78 24.8 49.4 97.8 248 494 737 978 Surrogate Std Cone. ug/mL 101 Surrogate Final Cone. ng/mL 498 AU Ain't Spiked mL 0.005 Calculated Concentrations of Standards in the 1.0 mL final solvent volume PFOS PFOSA PFOSAA EtFOSE Final Cone. Final Cone. Final Cone. Final Cone. ng/mL 5.00 ng/mL 5.01 ng/mL 5.00 ng/mL 5.00 10.0 10.0 10.0 10.0 25.0 25.0 25.0 25.0 50.0 50.1 50.0 50.0 100 100 100 100 250 250 250 250 500 501 500 500 750 751 750 750 1000 1001 999 1000 PFOSEA Final Cone. ng/mL 5.01 10.0 25.0 50.1 100 250 501 751 1001 M556 Std Cone. ng/mL 5.01 10.0 25.1 50.1 too 251 501 752 1002 Surrogate Std Cone. ug/mL 101 Surrogate Final Cone. ng/mL 505 AU Ami Spiked ml. 0.005 Sample used for MS/MSD: TCR99062-30 MS/MSD Cone, in the sample matrix PFOS PFOSA Final Cone. Final Cooc. ng/mL ng/mL 248 248 248 248 PFOSAA Final Cone. ng/mL 247 247 Initial Volume (mL): 1.00 EtFOSE PFOSEA MS56 Final Cone. Final Cone. Std Cone. ng/mL ng/mL ng/mL 247 248 248 247 248 248 Approx. Std Cone.: 50.0 ug/mL Ain't Spiked Vol. (mL) 0.005 Sample used for MS/MSD: TCR99O62-30 MS/MSD Cone, in the final solvent_______________________________Initial Volume (mL): 100_________ PFOS PFOSA PFOSAA EtFOSE PFOSEA M356 Std Cone. Std Cone. Std Cone. Std Cone. Std Cone. Std Cone. ug/mL ugraL ug/mL ug/mL ug/mL ug/mL 250 250 250 250 250 251 250 250 250 250 250 251 Approx. Std Cone.: 50.0 ug/mL Ami Spiked Vol. (mL) 0.005 Final Vol. (mL) 1.00 Toxl45 I" J * 000573 DILUTIONS SUMMARY SHEET Study: TOX145 Dilution Date/Analyst: 11/5/99 MCH Box #: 99-208 <*nlc/<}*5 ''P I sa m p le n u m b e r o r descrpition 9R03255-5m g/kg-Day 29 9R032S6-5mg/kg-Day 29 9R03257-5m g/kg-Day 29 9R03258-5m g/kg-Day 29 9R03259-5m g/kg-Day 29 -- ------ ---------------- 1:10 D IO D IO D IO D IO D IO L ilPr . . _ - 1: tit* . . . 1: N * . . - AO> jJJM _^T s rs'' s' / / ( V. Notes: D 10=100 u L sample + 900 u L M e O H . 1 Solvent/TN Num ber: M eOH T N -A - 3iY%k> Extraction Date/Analyst: MCH 11/3/99 M atrix/Timepoint: Rat Sera Day 29 1: jjA . _ . _ D IL U T IO N S 1: Comments Verified By - . Milk_________________ % L wV j\ ^ .. -. totVo . 1 .. 1 \ \ \ \ \ \ i \ 1 1 \ \ nK si/ Form C o m p jg tio n . Verified By I\ J -fl/i fa Extraction Worksheet ETS-8-6.0 ////5 -^ 5 Study * T O X -145 S urrogate Std FC Mix FC Mix FC Mix Com m ents Verified By Matrix R at Liver Approx, ppm approx.0 .5 ppm approx.5 ppm approx.50 ppm B o x # _ a a 2 1 J ______________ W K /D a y J J a y J B ___________ A ctu al/# / ppm actual * tfdtliX!. * ppm actual ppm actual -f?-Z # ppm /// D a te S p ik e d /A n a ly s t (U>Ut<t 9 - - C C V - /Y ,, /- 2 _ iflcJj'/C -M S- / -M SD- h/jA* 5 .0 ul 5 .0 ul 5 .0 ul / 7/ 10 ul 10 ul 10 ul /fa?- v 6 sV / ___ ___ \ /V -H 20B lk-142 -L iv e rB lk -1 & 2 -6 p p b -1 & 2 -1 2 p p b -1 4 2 -3 0 p p b -1 4 2 -6 0 p p b -1 4 2 -1 2 0 p p b -1 4 2 -3 0 0 p p b -1 4 2 5 .0 ul 5 .0 ul 5 .0 ul 5 .0 ul 5 .0 ul 5 .0 ul 5 .0 ul 5 .0 ul y / 2 ul 4 ul 1 0 ul 2 0 ul 4 0 Ul /. / .. / / / / / / 10 ul / / / / / h > / Humiifonfi A i i t ___!__ ! _ -6 0 0 p p b -1 4 2 5 .0 ul So 2 0 ul / -9 0 0 p p b -1 4 2 5 .0 ul 3 0 ul / ^ -1200ppb-142 5 .0 ul / / 4 ul Sam ple num bers and w eights noted on a separate page - add S'0 ul surrogate to all sam ples. / J -Tr--rr^P y) m) tO -- -------- -- -- 7y.jTM/ /? ... ... S * ..... am ou nt = /, /) ml 0,/i 3 g/ml L iv e r E x tr a c tio n M e th o d ___ E T S -8 -6 .0 D ate & In itials Vortex 15 Sec. Pipette Matrix, spike with appropriate surrogate or FC -M ix Volum e /,0 lt/S/9? __ ml Pipette 1 ml of 0 .5 M TBA. pH 10. dH = Std. # -/^SS u/<sJ+4 Pipette 2 ml of 0 .2 5 M N a ? C (V 0 .2 5 M NaHCO a buffer w . ff ywr \ Dispense 5 ml of methyl-t-butyI ether T N -A - 2 9V } S hake 20 min S h a k e r sp eed : 1/0fJ / C entrifuge 2 0 -2 5 min. C en trifuae S D eed: 7TdE> | R em ove a 4 ml aliquat of organic layer Put on Nitrogen Evaporator to dryness "t em p e ra tu re : R oo m 1 em p. Add methanol V o lu m e t .0 ml TN -A - Y- f ? 7 Vortex 30 sec. Filter using a 3cc B-D syringe with a 0 .2 urn filter into an autosam pler vial Cont. Cal. Verifications used sam e m atrix as for std curve. xS UN _ l __________ / un* a f r i I f f N T~ Uh " ^/ (Uci#- tilcyfr ====F=T* 'z 10/12/9 9 Draft Attachm ent A E TS -8-6.0 Extraction of P FO S from Liver Form Com pletion Vended Bi t i U A t t j * l h 1 000S75 Prep Dated): 11/3/99 Analyst!*): RWW Sample Matrix: Rat Liver Method/Revision: ETS-8-6.0 Target Analyte(j): PFOS, PFOSA Sample ID 9R03240/M/Day29/Control 9R03241/M/Day29/Control 9R03242/M/Day29/Control 9R03243/M/Day29/Control 9R03244/M/Day29/Control 9R03255/M/Day29/5mg/kg 9R03256/M/Day29/5mg/kg 9R03257/M/Day29/5mg/kg 9R03258/M/Day29/5mg/kg 9R03259/M/Day29/5mg/kg Sample Weights/ Volumes 0 ^ I? / . / _ - /( iS Initial Wt g _.L A U a // /, A J -5 /,//? $ h jy -/ /.fiZ tO /, / 6 0 ? /r fy A Y /? MQ Water ml 5 ml 5 ml 5 ml 5 ml 5 ml S ml 5 ml 5 ml S ml 5 ml Study Number: TOX145 Equipment Number: Final Solvent & TN Number: MQ Water Matrix Blank/ldentifier: Rabbit Liver/99086-l3-S Box: 99-211 Verified By: Comments ------- -- ----- ----------- y t fjc , / d i --------------- ----------------------------- ---- ---- ) ~~ ifM 7 7 _ _ _ _ _ ------------- -- r Summary of method: Notes: R e vie w Date Form Approved by/Date:, Weight Volume Sheet-I01299.xls Form Completionn // Verified By M M n /uH/r B O O S T 'S Ion Pair Standard Curves-Tusues r t p , , / - ///y /p p Prep Date(t): Anaiyat(i): Sample Matrix: Method/Reviaion: Target Analyte(>): Box Number: 11/4/99 RWW A <-0 Rabbit Liver ETS-8-6.0 See below 99-211 // FC Mix Std Approx. 0.500 ppm: FC Mix Std Approx. 5.00 ppm: FC Mix Std Approx. 50.0 ppm: Surrogate Std Approx. 101 ppm: 99086-44-3 99086-44-2 99086-44-1 99086-13-11 Actual Concentrations o f Standards in the FC Mix PFOS PFOSA EtFOSE-OH Std Cone. Std Cone Std Cone. ug/mL ug/mL ug/mL 0.5004 0 5000 0.5000 0.5004 05000 0.5000 0.5004 0.5000 0.5000 0.5004 0.5000 0 5000 0.5004 0.5000 0.5000 5.004 5.000 5.000 5.004 5.000 5.000 5.004 5.000 5.00Q 50.04 50.00 30.00 MS56 Std Cone. ug/mL 0.5000 0.5000 0.5000 0.5000 0.5000 5.000 5.000 3.000 50.00 Calculated Concentrations o f Standards in the sample matrix PFOS PFOSA EtFOSE-OH M5S6 Std Cone, Std Cone, Std Cone, Std Cone, "g/g "r t g/g a r t 6.14 6.13 6.13 6.13 12.3 12.3 12-3 12.3 30.7 30.7 30.7 30.7 61.4 61.3 61.3 61.3 123 123 123 123 307 307 307 307 614 921 1228 613 920 1227 613 920 1227 6(3 920 1227 Study Number: TOXI45 Equipment Number: Final Solvent A TN Number: MeOH/TN-A-2997 Rabbit Livr/99086-13-S M570 Std Cone. ug/mL 0.5000 0.5000 0.5000 0.5000 0.3000 5 000 5.000 5.000 50.00 M370 Std Cone, art 6.13 12.3 30.7 61.3 123 307 613 920 1227 Blank liver initial density (g) for curves: Final solvent volume (m l.) for curves: 0.163 1.000 MeFOSE-OH Std Cone. ug/mL 0.5000 0.5000 0.5000 0.5000 0.5000 5.000 5.000 3.000 50.00 POAA Std Cone. ug/mL 0.5000 0.5000 0.5000 0.5000 0.5000 5.000 5.000 5 000 50.00 PFHS Std Cone. ug/mL 0.5000 0.5000 0 5000 0.5000 0.5000 5 000 5 000 5 000 50.00 All Ain't Spiked mL 0.002 0.004 0.010 0.020 0.040 0.010 0.020 0.030 0.004 All Density 8 0.163 0.163 0.163 0.163 0.163 0.163 0.163 0.163 0.163 All Vol. mL 1.000 1.000 1.000 1.000 1.000 1.000 1.000 1000 1.000 MeFOSE-OH Std Cone, "g/g 6.13 12.3 30.7 61.3 123 307 613 920 1227 POAA Std Cone, "g/g 6.13 12.3 30.7 61.3 123 307 613 920 1227 PFHS Std Cone, ng/g 6.13 12.3 30.7 61.3 123 307 613 920 1227 Surrogate Std Cone. ug/mL 101 Surrogate Final Cone. >g/g 3098 AH Ain't Spiked mL 0.005 Calculated Concentrations o f Standards in dm 1.0 mL final solvent volume PFOS PFOSA EtFOSE-OH M556 Final Cone. Final Cone. Final Cone. Final Cone. ng/mL ng/mL ng/mL ng/mL 1.00 1.00 1.00 1.00 2.00 2.00 2.00 2 00 5.00 5.00 5.00 5.00 10.0 10.0 10.0 10.0 20.0 20.0 20.0 20.0 50.0 50.0 50.0 50.0 100 100 100 100 150 130 150 150 200 200 200 200 M570 Final Cone. ng/mL LOO 2.00 500 10.0 20 0 500 100 150 200 MeFOSE-OH Std Cooc. ng/mL 1.00 2.00 3.00 10.0 20.0 50.0 100 150 200 POAA Std Cone. ng/mL 1.00 2.00 5.00 10.0 20.0 50.0 100 150 200 PFHS Std Cone. ng/mL 1.00 2.00 5.00 10.0 20.0 50 0 too ISO 200 Surrogate Std Cone. ug/mL 101 Surrogate Final Cone. ng/mL SOS AU Am't Spiked mL 0.005 Sample used for MS/MSD: MS/MSD calc. In matrix PFOS Final Cone. ng/g 295 295 Sample used for MS/MSD: MS/MSD calc. In solvent PFOS Final Cone. ng/g 50.0 50.0 9R03240 Initial W t (g): 1.020 PFOSA EtFOSE-OH Final Cone. Final Cone. ng/g "g/g 295 295 295 295 M5S6 Final Cone. ng/g 295 295 Initial Volume (mL): 5.00 M570 MeFOSE-OH Final Cone. Sul Cone. ng/g ng/g 295 295 295 295 6.00 POAA Std Cone. "g/g 295 295 9R03240 Initial W t < PFOSA Final Cone. "g/g 50.0 500 EtFOSE-OH Final Cone. ng/g 500 500 M5S6 Final Cone ng/g 30.0 500 Initial Volume (mL): 5.00 MS70 MeFOSE-OH Final Cone. Std Cone. ng/g "g/g 50.0 50.0 500 50.0 POAA Std Cone. ng/g 50.0 500 Approx. Std Cone.: 5.00 ug/mL Ain't Spiked (mL) PFHS Std Cone. g/g 295 295 Density Approx. Std Cone.: 5.00 ug/mL PFHS Std Cone. Am t Spiked (mL) ng/g 50.0 50.0 Final Vol. 1.000 IPSE- I0259LV-99086-44- l.xls 000577 DILUTIONS SUMMARY SHEET Study: TOX-145 Dilution Date/Analyst: SAL 11/9/99 Box#: 99-211 Solvent/TN Num ber: MeOH T N -A - 3 ? Extraction Date/Analyst: RW W 11/4/99 M atrix /T im e p o in t: Rat Liver Day 29, G rp 6 sam ple num ber DILUTIONS or dcscrpition l : | 0 0 1: 1: 1: t: 1: 1: Comments 9R03255/M/Day29/5mg/kg 0 1 0 0 V /P l 9R03256/M/Day29/5mg/kg 9R03257/M/Day29/5mg/kg 9R03258/M/Day29/5mg/kg 9R03259/M/Day29/5mg/kg *r I Vf Verified By < Y ______ ^ ________ 1 Z/ br -Q I n .... *4 , tL. 1 I 000578 No,es: D io o r r u u U /o x J S iu ^ U /M3f7 Form Com pletion .. \/prifipH Ru U / t A h Iq / o ^ FACT: DATA REVIEW SUMMARY FORM p l* J z . Date: Data Analyst: Data Review Sign-OfT ' Analyst Review Name / Date: A?4>/W _________ FACT Study#: 7S)U<J / Matrix/Timepoints; H -/S v c -~Div / j 4- Pad**ij list ~**l7 7 /7 ? SSE. T1eKcOhInJiKcIaIl RRBevTiWewW . Name/Date: {/) loJ^&jQQ Sample List: Set-up Analysis Date/Analyst l "/ n / 7 t M l*H Quality Assurance Review Name / Date:_____________ Data E ntry:. ,,LAC l lu lft Instrument S>4> O 7ol99 7 Anatvte: oAA ( C H f f Acceptable Linear Ranse: A " See <liinju.>i4s LOO: A/A Extraction Blank A/A Comments / Justifications 0 A C u -'l* . IUCS A /~ er/* t/tjL 'll* . A s L i ___ J . . ? O A * ~ ____ / g 0 * /y J t o J -Ear h a k i K j a / e r a . a tu jc RA2: AIA Calibration Checks: A lA MS/MSD: &Ac 0 rT Data Status: ern Matrix Blank ItA Stl_ ^ 9 3 ^ > L p ailiJ - U tS c / r t ^ f / lte a .U A / ' / A /< f D u /s z/e . - f L //ft*- Att/ryc___ e t 4 L .. cg r u c ___ s ^ & s ___t W y o t * * r /g ___ tr * b * /< T a s u / m & Analyte: T f o S ( Q iz ^ 4 L t u a f f > A L s / / t J A j -A L t / b S / Acceptable Linear Range: LOQ:. l ^ L R*2: & 7 f g M > M ffL Extracted Blank J fs s 4 L * . L& i Matrix B lank /* s j -La - L o ti S a -b JiU s f u iL y * 4 4 L S a m J tL t A a J A tjj arm. C ouds d u d ustn OuJe/Je___ 4 L rS-Hjt <=4 9ucL,J',4aJi<<-. --T m e J r f Calibration Checks: /L Jim * ~ /i 4 * /L "A ^ u*_j^.L-A>ssl _____ MS/MSP: f)V _________________________________________ k K r t J y g ^ e e i -/Ce- 4 L C aute* lorie a iL S * -. Data Status: D . i u W t iNflAlA fio tti W n i JL a u J iiJ c 4 L K A H jy . w Analyte: ^ F o S fi ( fti-3 ) Acceptable Linear Range: 4-93 rj>l> * ?3n,L__________ LOQ: 4 -9 3 obL______ Extracted Blank: I n s 4 L 0<S r *2 _ Matrix Blank jess 4 b u - lo Q Calibration Checks: OK - L u * . --/ 3 % ------> /V MS/MSD: DaUSatus: _L Kl ,IA C 'lolx-hh t L a M titf L am-L L J Ja.h? /y A ijL I c i t i k < d E l ^ __ I ________ PQA &.m mX * * <^c A*%Q M c a * 3 r Q i l r f f a t i j P l J A -IMl U U d ) M u O C A M u e a S ^ * ^ p^a/ud(fr *(d ent* uajtd. fis AxnjjKLpD A X a o , A J .a ^ a .U ^ Y ' \ k * 4 i i u t U Q 1 \ X a a _____ Y *>** _______ 000579 FACT: DATA REVIEW SUMMARY FORM T S " / * ' / * * f> 2 - Date: /VWfy___________________________ , Data Analyst: FACT Study#: 3*S _______________________ Matnx/Timepoints: / * / -ChJtJ * - fit/. % /tfX Sample List: h / 7 l 1 L _______________________________ Set-up Analysis Date/Analyst: . / ? / ? / f f MfiftJ Instrument: ft'auf, 02 H I f Data Review Sign-Off Analyst Review Name / Date: 3 ~a < / A ,/ ________ Technical Review N am e/D ate:__________ u . |)fiy. l f tf 3- VC L o f Z t M Quality Assurance Review Name / Date:___________________________ Data Entiy: lAc IoIh I m _______________ Comments / Ju stifica tio n s:____________________________ Analyte: S C cH 'f )(2> Acceptable Linear Range: H a LOO: AC** Extraction Blank: H a RM: HA Matrix Blank: H a Calibration Checks: HA MS/MSD: ~~------- Data Status: s~--' l ^ l e r t u s .f S / CLh -a , fia u .K .- f s / C ____________ __ Aff jS ~ y l t i . r v < s . C aJ ChcJu h J /eutaJtas p t &>% or/< K i. ^ J a S ,0/ * ,i n __________________________________ 0005S0 - .... -, ' . * . .1 Quantify Ca^ouad l u y Report TOX145-rae aera, Any I & 4, control a dosa- ext. 10/19/99 E U copia Lit: C:\10LSSLntX\soup-rata.proVBa9lcJMtl01999b Last nodiflad: Wad Oct 20 07:37:23 1999 Method: C:\IOSSLnac\aoup-rats.pro\MaehSBU01999b Last Modified: Wad Oct 20 07:34:41 1999 Job Coda: Printed: Wad Oct 20 01:00:10 1999 Propound 1: P O U (Cbl) Naan 1 101999012 2 101999013 1 101999014 4 101999015 5 101999016 6 101999017 7 101999018 8 101999019 9 101999020 10 101999021 11 101999022 12 101999023 13 101999024 14 101999025 15 101999026 16 101999027 17 101999028 18 101999029 19 101999030 20 101999031 21 101999032 22 101999033 23 101999034 24 101999035 25 101999036 26 101999037 27 101999038 28 101999039 29 101999040 30 101999041 31 101999042 32 101999043 33 101999044 34 101999045 35 101999046 36 101999047 37 101999048 38 101999049 39 101999050 40 101999051 41 101999052 42 101999053 43 101999054 44 101999055 4S 101999056 46 1019990S7 47 101999058 48 101999059 49 101999060 SO 101999061 51 101999062 52 101999063 53 101999064 54 10199906S SS 101999066 56 101999067 57 101999068 S8 101999069 59 101999070 60 101999071 61 101999072 62 101999073 Seriellst Teat MeOH H a n k MaOH Blank MaOT Blank TOX14S-RBS10199-H2O Blank-11. SCX TOX14S-R8S10199-Sere Blank-11. SB1 T0X145-RTS10199-Sera Blank-11. S U TOX14S-RTS10199-Sera Blank-12. SSI TOX145-RBS10199-5ppb-ll, SEE TOX145-RBS10199-lOppb-11. SEE 7OZ145'RBS10199-25ppb-ll. SEE TOS145-RBSlQ199-50ppb-ll. S U TOS14S~RAS10199-100ppb-ll, SEE TOX145-RBS10199-250ppb-ll, S U TOU45-RBS10199-S00ppb-ll, S U TOX145-RU10199>750ppb-ll. S U TQZ14S-RBS10199-1000ppb-ll, S U MaOH Blank TCQQ45-RTS, 9R03230M. Dyl-. Control.-10/19/99 S U TOZ14S-RTS, 9X03231M, Dyl. Control.-10/19/99 S U TCQDL45-RTS, 9R03232M, Dyl, Control.-10/19/99 S U TQZ145-RTS, 9E03233N. Dyl. Control.-10/19/99 E U TOX145-RTS, 9R03234M. Dyl. Control,-10/19/99 S U TGZ145-RBS10199-250ppb-CCV-ll-l, S U MaOH Blank TOX145-RTS. 9R03235M, Dy4. Control,-10/19/99 S U T0X145-RTS. 9R03236M. Dy4. Control.-10/19/99 SEX TOX145-RTS. 9R03237M. Dy4. Control,-10/19/99 S U TOX145-RTS, 9R0323SM, Dy4. Control.-10/19/99 S U TOX145-RTS, 9R03239M. Dy4. Control,-10/19/99 S U TOZ145-RBS10199-250ppb-CCV-ll-2, SEE MaOH Blank TOX145-RTS10199-2S0ppb-MS-ll. 10/19/99 SEE TOZ145-RTS10199-2S0ppb-MSD-ll. 10/19/99 S U T0X145-RTS. 9R03245M. Dyl. 5 ng/kg 10/19/99 S U TOX14S-RTS. 9R03246M, Dyl. 5 ng/kg 10/19/99 S U 70X145-RTS. 9R03247M. Dyl. 5 ng/kg 10/19/99 S U TOX145-RBS10199-250ppb-CCV-ll-3. SEE MaOH Blank TOX145-RTS, 9R33248K, Dyl. 5 ng/kg 10/19/99 SEX TOX145-RTS, 9R03249M. Dyl. 5 ng/kg 10/19/99 S U T0X145-RTS, 9R03250M, Dy4. 5 ng/kg 10/19/99 S U TOX145-RTS. 9S3251K. Dy4, 5 ng/kg 10/19/99 S U TOX145-RTS, 9R03252K. Dy4, 5 ng/kg 10/19/99 SEE TOX145-RBS10199-25Cppb-CCV-ll-4. S U MeCH Blank TGX145-RTS, 9?.0::S4-1M. Dy4, S ng/kg 10/19/99 S U TOXI4S-RTS, 9?.:i:ii-2M. Dy4. 5 ng/kg 10/19/99 S U t o x :45-r b s i o :53-:s :ppb-ccv-ii-i, see MeCH Blank TCX145-RBS10199-H2O Blank-11. SEE TOXI45-RBS10199-Sera Blank-11. SEE TCX145-RTS10193-Sera Blank-11. SEE TOX145-RTS10199-Sera Blank-12. SSE TOX14S-RBS1019-Sppb-ll. SEE TOX14S-RBS10199-lOppo-11, S U TOX145-RBS10199-2Sppb-11, SEE TOX145-RBS10199-S0ppb-ll. SEE TOX145-RBS10199-100ppb-ll, SEE TOX14S-RBS10199-2S0ppb-ll. SEX TCX145-RBS10199-SOCppb-ll. SEE TCX14S-RBS10199-750ppb-ll, S U TOXI4S-RBS10199-100Oppb-11, SEX Type Standard Standard Standard Standard. SfaMlarrf Standard Standard Standard Standard QC QC QC QC QC Standard Standard Standard Standard Standard Standard Standard Standard Standard Std C O M 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 ET 7.085 7.123 7.121 7.112 7.084 7.111 7.109 7.100 7.112 7.110 7.111 7.112 7.111 7.090 7.111 7.110 7.086 7.113 7.089 7.133 7.112 7.129 7.112 7.106 7.105 7.132 7.123 7.090 7.111 7.112 7.107 7.104 7.090 7.108 7.103 7.110 7.113 7.110 7.113 7.111 7.109 7.129 7.110 7.091 7.113 7.134 7.132 7.111 7.126 7.111 7.111 7.107 7.110 \ ) dV C, \ r a l} n a l u k . ' floi- u n d . Ac lbk `h<i Ji* __ j> (*4 Area Plag* Cene. kDaw 37 MM 38 MM 34 MM 38 MM 35 bb 42 bb 33 bb 42 bb 39 bb 39 bb 51 MM 42 bb 60 IM 30 MM 37 bb 36 bb 42 Ml 43 MM 34 MM 29 bb 37 MM 34 Ml 33 bb 30 MM 40 Ml 56 Ml 35 bb 308 bb 425 bb 360 bb 42 bb 291 bb 340 bb 210 bb 209 bb 260 bb 31 bb 24B bb 234 bb 39 bb 28 MM 38 bb 28 bb 44 MM 31 Ml 37 Ml 34 Ml 40 Ml 37 Ml 45 Ml 37 Ml S3 bb 64 bb 0.88 0.91 0.81 0.90 0.83 0.99 0.77 1.00 0.92 0.93 1.21 1.00 1.41 -12 -9 -19 -10 -17 -1 -23 0 -8 -7 21 0 41 0.71 0.87 0.85 1.00 1.02 0.81 -29 -13 -15 -0 2 -19 0.68 0.88 0.81 0.77 0.72 0.96 -32 -12 -19 -23 -28 -4 1.32 0.83 7.28 10.06 8.52 1.00 32 -17 628 906 752 -0 6.88 8.04 4.97 4.93 6.15 0.73 588 704 397 393 515 -27 5.88 488 5.55 455 0.92 -8 0.66 0.89 0.66 1.04 0.73 0.87 0.81 0.95 0.88 1.07 0.87 1.26 1.51 -34 -11 -34 4 -27 -13 -19 -5 12 7 -13 26 51 cup 020199: Qunatifiad and printed fry ina on 10/19/99 T, tf *i <r- A i3 4 ui ^ a- "a os o - -5 Vo? -o loeooc ><r>*Hmp*it* Hh 300000*0 -? 1-an--\ - no nmn* oopp**i Nr- 12 r n 1 1*1N N h h h o h na an nnnAapnnP kaHaiAi< >o o o n a >QOOHM<i * haaisasiaaaaaaaaiauiaaiaaaaaaiaaaaaaaaaaaaaiaaaaianiaaaaaaai M HHi Hai Hi ^ainooar-at Hr<aiHAioAnHt<Hi ncc HH HrtHr1hHNMHi 4 nnanae >t'00AatnHHna< E? aneoeweaonOHHi> M MoNN Manmn*nmN*n*Hmn*n ni nmnmra loh cafnoafairn tn a n a a a t Mf i aonwoi n_ Hanon^_o_n_Hin naamni nn iHf l a irAtawi fHl ioAaa a m nnrtnnnnNnnnnnn" nnnnnnnnn nnnnnnnnnnnnnnnnnn -r-r-p-p-p-p-p-p 30 0 00 AOOOO a n aooooooo 5 5 5 :5 SHSSH .................e s s 55 MMM Sh h m v tm m ... _________ r-4 -- r4 M M M M M M M W ooooo HHHHH '. ' . B HHHHHM OOOOO J55Uit rt cacea i OOOOOH H ooooo HtHHHiH '.S HHHHHM -o-o-o-o-o u muu u 4J*J* i U U p caacci OOOOOUUH a HHH HHr SW >000 ooc VHHHM OHNVN - ; SST Hhirtin H i > MUHHH lUmUhMhmwBeimnnmm km\ HHHf i M j u io ta ai Ka kaaau u o M0 Ou- bI ..........i, uu o, ut uo uu o vi u oo in u XMt i Mi i xi i i i f ' Hni nhH 1i i i i >i t i i i i i ft>iAa>ioi o< o< O' ooooooooooooo HHHHHb V ss *:* r a~ o nnnrrn rr ri n ri if nnnnnr nnnnn i oooooo K K I< tt et or- e MSHHH5 HH^^ (5 SiV ??V V r....r.....r.....y.....r...4n, a r ....................* .................ft ssi sM in .. s3S i Mi nvi Mwaww la a na n an a 1K1KK2KK H i H H H I t l l l l l l l l l l l H I t l l l l H l l i t i I H I I I I I l H l I I I I I H I I H I II R M N i n i A i n i f t n i f t i n i i i i n i l n i n i n i n i n i n a i n < n i n a i i i i n X i n i n l |l X |' ' i A i n S-- lfHt a X X H* *H *H *H*H*n *H *H*H*H*H*H*H HoHoHoHo Ho oH X H* H* n* H* -*i H* S H*H*H*.*i H* H* M* *^ i*f *i n*H*f _i - .*i .*- *. i _r - '*f ** -*' f O O Q X X X X X X x X X X x X X Q X K X X x x O x x x X x x o X X X X x x u : : x x x x x i x x : ; - 8 8 8 8 8 8 8 8 8 8 8 8 8 1 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 8 4 8 8 8 8 8 8 * 8 8 8 * 8 8 8 8888888888 0n o n< o * r a o Hn n M p - a ooooooooooooo o o o o o o iw f'a O H n H a ifl o'3i 0n n0n0n0H0a0a 0a a0a0a0a A 0a r-a a0i0n o 0i n0i H 0n n n H i n p a '- i n n n0a0t0f i0a 0i n0i 0A 0i A000 0 0 a ypaAOHnn pppr* oo aot soi ooeoi ooooi ooc ho*o A li H r l H H H H n HHHi ooooooooooc KlriHrlrlrlrlrlHMHFAlAf1AHAf1AAHrA1AH AAAAAAAAAAAAAAAAAAAA rlHHHHHHHHH 3OOOOOOOOOOOOOOOOOO0 3 0 0 0 0 0 0 0 0 0 C 300 0 0 0 0 OOOOOOOOOO I HHrl HHH iapnnoH nnain*paO H N n4 p a o h n N 00 Q u a n tify Ciazio unil l u a n r y H*porc TOX145-rat sor*, day 1 6 4, cor.croi a dono* *t. 10/19/99 aol Lit: C:\MAS8CTKX\*up -rat*.pro\SauplaDB\101999b U S t nodifiodi Od Oct 20 07:37:33 '.99 aaathod: Ci\KR8St,Elix\*o\ir-rat.pro\llaehDS\mf9b u a t nodiflod: wod Oct 20 07:3c :48 1999 Job Coda: Printad: od Oct 30 04-0E'.V0 i9 Ccnoeuad 3: PPOSA (Ch3) MM X 101999012 2 101999013 3 101999014 4 101999015 S 101999016 6 101999017 7 101999018 S 101999019 9 101999020 10 101999021 11 101999022 12 101999023 13 101999024 14 101999025 15 101999026 16 101999027 17 101999028 19 101999029 19 101999030 20 101999031 21 101999032 22 101999033 23 101999034 24 101999035 25 101999036 26 101999037 27 101999038 29 101999039 29 101999040 30 101999041 31 101999042 32 101999043 33 101999044 34 101999045 35 101999046 36 101999047 37 101999048 39 101999049 39 101999050 40 101999051 42 101999053 43 101999054 44 101999055 45 101999056 46 101999057 47 101999058 48 101999059 49 101999060 50 101999061 51 101999062 52 101999063 53 101999064 54 101999065 S5 101999066 56 101999067 57 101999068 58 101999069 59 101999070 60 101999071 61 101999072 62 101999073 awplallst Text MaCK Blank lteOK Blank MaOH Blank TOX14S-BBS101; -h :: Blank-11, S U TCXUS-RBSlOl? -Sara Blank-11. SSt TCXUS-RTSIOI -Ser* Blank-11, S U TCXU5-RTS101- -Sera Blank-12, SEE t o >:i45-r b s i o :: -Si-tb-ll. SEE TCiiliS-RBSlO:"- -1-tpb-ll, SEE TCXL4S-RBS131; -Cjpb-U. SEE t c ::i45-r b s i o i : -Sltpb-ll, SEE TOX14S-RBS1019 -lOOppb-11. SEE TOX145-RBS101 ?-253ppb-ll, S M TOX14S-RBS101r -5c:ppb-n, s u TQX14SfcBSlQl9}-7S3ppb-U, S U TOX145-R35101S 3-10J0ppb-ll. S U MaCK Blank TOX145-RTS, 9R03230M. Dyl. Control.-10/19/99 SIS TOX145-RTS, 9RJ323W, Dyl. Control,-10/19/99 IBS TGX14S-RTS, 9R33232M. Dyl. Control,-10/19/99 S M TOX14S-RTS. 9R03233M, Dyl, Control,-10/19/99 SBS TCX145-RTS, 9R03234K, Dyl, Control.-10/19/99 SBS TOX145-RBS1019 3-2: 3ppb-CCV-ll-l, S U MeCH Blank Tc::ii5-RTS. 9? 322SM. Dy4, Control,-10/19/99 S U TC.-45-RTS, 9R23236M. Dy4, Control.-10/19/99 S U TC:i45-RTS. 97 32*7M. Dy4, Control,-10/19/99 S U TC..145-RTS, 9: 3UM. Dy4, Control,-10/19/99 S U tc 5-r t s , 9" 32:JM, Dy4. Control.-10/19/99 S U t c :::i5-r b s i o : - Z I ppb-CCV-11-2, SEE Me-H Blank Tc:-:i45-RTS10ir- -UJppb-MS-11, 10/19/99 S U TC"145-RTS10::- -CICppb-KSD-U, 10/19/99 S U TC::i45-RTS. 9.- 3::s m , Dyl. 5 ng/kg 10/19/99 S U Tc::i45-RTS. 9; 32.-JH, Oyl. 5 ag/kg 10/19/99 S U TC::i45-RTS. 97. 3247M. Dyl, 5 ag/kg 10/19/99 S U t c ::i45-r b s i o i :- -2 5Cppb-CCV-ll-3, S U Ml ;H Blank TC 'll45-RTS, 9* 3C4'M. Dyl, 5 ag/kg 10/19/99 SEE Tl 1145-RTS. 97. Dyl. S ag/kg 1Q/19/99 S U j2:,M, Dy4, 5 ag/kg 10/19/99 SBB TC US-RTS, 9" 3:S_M . Dy4, S ag/kg 10/19/99 SB1 V liS-RTS, SrtUM. Dy4. 5 ng/kg 10/19/99 S U T~ .'.5-RSS101 :;ppb-CCV-ll-4. SEE Mv : Blank TC :;S-RTS, 32r4-1M, Dy4, 5 ag/kg 10/19/99 SEE TC 145-RTS, t Oy4, 5 ag/kg 10/19/99 SEI T " H5-R3S101 :ppb-ccv-n-i, s u Blank TC::i45-RBS101. -h :j Blank-11. S U t c :::;s-r b si c i ' : - * Blank-11. SEE TCI.145-RTSlo: ' -r.ra Blank-11, SEE TC .11S-RTS101 -s .a Blank-12. S U T Z HiS-RSSlOl .b-ll, SEE TC" 14S-RBS101 ppb-l i , s e e T `.-:145-R9S10: -l:spb-ll, SEE TC. liS-RBSlOi: - S J p p b - l l , s u T:...45-RBS101' -l.lppb-n, SEE T ' .1145-RBS101r -2 5 Dppb-11, SEE T. 145-RBS101* 5 .'3 p p b - U . SSB TOI 145-RBS1011- '5 :ppb-ll, S U TOI 145-RBS101 -1J)0ppb-ll, SBB Typa Standard Standard Standard Standard Standard Standard Standard Standard Standard QC QC QC QC QC Standard Standard Standard Standard Standard Standard Standard Standard Standard Btd Game 4.93 9.77 24.80 49.30 97.70 248.00 493.00 736.00 977.00 248.00 246.00 248.00 248.00 248.00 4.93 9.77 24.80 49.30 97.70 248.00 493.00 736.00 977.00 ** 7.836 7.806 7.853 7.833 7.839 7.822 7.834 7.808 7.813 7.110 7.802 7.814 7.811 7.809 7.814 7.813 7.877 7.836 7.834 7.808 7.832 7.837 7.812 7.854 7.856 7.837 7.852 7.858 7.852 7.806 7.854 7.789 7.803 7.791 7.790 7.814 7.809 7.881 7.805 7.791 7.804 7.789 7.814 7.856 7.813 7.792 7.811 7.857 7.854 7.851 7.833 7.859 7.814 7.613 7.811 7.813 7.805 7.813 7.791 7.786 7.811 i m Plaga 2725 MN 539 MC 294 MK 171 MK 154 Mt 159 MM 145 MM 1074 MM 2036 MM 5196 MM 9515 MM 16241 MK 49679 MM 100839 IM 117401 MMX 149225 MMX 993 MK 363 Ml 226 MM 147 MM 150 Ml 142 Ml 49041 Ml 312 Ml 168 Ml 139 MC 167 MM 146 Ml 136 MM 43165 MM U S NM 46811 MM 52881 MM 52155 Ml 87504 Ml 51116 dd 49904 MM 364 MM 67032 db 55570 MK 11759 dd 151S8 MK 46625 M( 307 Ml 12235 bd 11895 MM 50283 MM 348 MM 145 MM 126 MM 120 MM 148 MK 1139 MM 2063 Ml 5615 MK 10041 MM 18028 Ml 51069 MM 100103 IM 122134 MMX 153334 KKX Ceno. %Dav 13.20 2.28 1.06 0.45 0.36 0.39 0.32 4.96 1 9.76 -0 25.54 3 47.10 -4 80.69 -17 247.65 -0 503.11 2 565.80 -20 744.71 -24 4.55 1.41 0.72 0.33 0.34 \\ \ \ 0.30 244.47 1.15 -1 \\ 0.43 0.29 0.43 \\ J0.32 0.27 215.13 - U /y 1.17 243.32 1 263.64 260.01 436.52 254.83 248.78 0 V\\' 1.51 334.30 277.07 58.31 75.28 232.41 -6 1.13 60.69 58.99 250.67 1.33 0.32 1 1 //// 0.23 0.19 0.34 5.28 7 9.90 1 27.63 11 49.73 1 89.61 -8 254.60 3 499.43 1 609.44 -17 765.23 -22 r< s io| 4 ^ oup 030199: Quantified and p r . : by la on 10/19/99 000583 Quantify Caapound M u r y Mpc:-. TOX145-rat sara. day 1 & 4, cor.troi a dosa- axe. 10/19/99 S R Sanpla fclat: C:\MRSl,Yia\sovr-raw.pre\Sanplalia\101*99b baa nodiflad: Wad Oct 30 0 7 : " : if Nattaod: c:\KbSSLYNX\soup-rata.praMlathDBM019f9b baa nodlfiad: wad Oct 20 07:3*:8 1999 deb Coda: Friatad: Wad Oct 20 04:Ci-.l0 1999 4: IS (CM) 1 101999012 2 101999013 3 101999014 4 101999015 S 101999016 6 101999017 7 101999018 8 101999019 9 101999020 10 101999021 11 101999022 12 101999023 13 101999024 1 101999025 IS 101999026 16 101999027 17 101999028 18 101999029 19 101999030 20 101999031 21 101999032 22 101999033 23 101999034 24 101999035 25 101999036 26 101999037 27 101999038 28 101999039 29 101999040 30 101999041 31 101999042 32 101999043 33 101999044 34 101999045 3S 101999046 36 101999047 37 101999048 38 101999049 39 101999050 40 101999051 41 101999052 42 101999053 43 101999054 44 101999055 45 101999056 46 101999057 47 101999058 48 101999059 49 101999060 50 101999061 51 101999062 52 101999063 S3 101999064 54 101999065 55 101999066 56 101999067 57 101999068 58 101999069 59 101999070 60 101999071 61 101999072 62 101999073 Saaplaliat Ta.t MaOH Blank MaOH Blank MaOH Blank TOX145-RBS10L ?-h :d Blank-ll. SEE TOX145-RBS10: >-Sera Blank'll. 8KB TOJQ45-RTS10; -E-ira Blank-11, S R TOX145-RTS1S: '.--Sera Blank-12, S R TOXl-i5-RBS101 '-Srpb-ll. S R TOXliS-RBSlO: >-::rpb-n. S R t o x i ; 5 - r b s : o: -rijpb-ii, sec TOX145-RBS:o: :?pb-ll, SEE T0xi;5-RBSi:: -)-::appb-n. sek TOXI5-BBSIC1-)-:E3ppb-ll, SEE TOX145-RBS1C! ^5:0ppb-ll. SEE TOX145-RBS10:i - 7 Jppb-11, SEK TOX15-RBS10; 9-i:Q0ppb-ll, S R MaOH Blank TOH4S-RTS, i; 3323QM. oyl. Control,-10/19/99 S H TOXK5-KTS. 9: 332UM, Dyl, Control. -10/19/99 S R TOXU5-RTS, 33232M. Oyl. Control.-10/19/99 S R TOX145-RTS. 5? 33233K. Oyl, Control,-10/19/99 S R TOX145-RTS, E-:33224M, Oyl, Control,-10/19/99 S R T0X24:-RBS10I-3-223ppb-CCV-ll-l, S R MaOH alank TOX145-RTS. 9* 22 5M. Dy4, Control.-10/19/99 S R TOX145-RT3. .32:M, Dy4, Control,-10/19/99 S R TOXli >-RTS. 2 2 : '?M, Oy4, Control,-10/19/99 S R TOXI4 ;* R7 3 . ' '222 ; M , Dy4, Control.-10/19/99 S R TOXI4` -RTG, ( 3::-M, Dy4, Control,-10/19/99 S R TOXI4 i-RoSlOl ; -2 2 'ppb-CCV-11-2, S R MaOH 3lar.< TOXI45-RT51C1 ::ppb-MS-ll, 10/19/99 S R TOX14 5-RT31C1 -:::ppb-KSD-ll. 10/19/99 S R TOX145-RTS. 9 : 3 2 4 ; H , Oyl. S ng/kg 10/19/99 S R TOX14 3-RTS, c ' . Z i i x , Dyl, 5 ag/kg 10/19/99 S R TOXli 5-RTS, 5.- 33247M, Oyl, S ag/kg 10/19/99 S R TOXI4 5-RB310: .- - 2 : 3ppb-CCV-ll-3, S R MaOH 31an< TOXI4 3 -RT3. : : 22 42M, Oyl. S ng/kg 10/19/99 R S TOXI4 i-RT3, ? ' -3243K, Dyl. 5 ng/kg 10/19/99 S R TOXI4 ' -RT3, 9 SR T0X14:-RTS. : Dy4. 5 ag/kg 10/19/99 R S T0X14:-RT3. < Dy4, S ag/kg 10/19/99 S R TOXI4 : -RSG1C. -::.:ppb-ccv-n-4, S R MaOH lar .k TOXI4 " - R7S. :::4-lM, Dy4, 5 ag/kg 10/19/99 S R TOXI4 -R7 . '> 1 : 1 - 2M. Dy4, 5 ag/kg 10/19/99 S R tox14-:-?.s : i ; . :ppb-ccv-n-i, S R MaOH - L a r . . . toxi 4 r l : : : : 7 Blank-ll, SEK t o x i 4 - s : : : : : -Sera Blank-ll. S R toxi 4 Blank-ll, SEK t o x i 4 -3T_:: -Tira Blank-12. S R t o x i 4 -RS.-::. -5" :b-ll, SSE TOXI 4 :-R 3 1C. -1 - pb-11, SEE t o x i 4z - r l s : : : - 2 : Dpb-11, SEE tox 14-:*r e .:i o : -52ppb-11, SEE TOXIC-Rs'lO. -1 ; Jppb-11, SEE TOXI4:-RJ1C. --:;3ppb-n. see TOX145-REJ1C1 -iCJppb-11. SEE TOX14;-0.-1O: -'Eppb-ll, SEE TOX14--R2S10: ' J0ppb-ll. SEE typa Standard Standard Standard Standard Standard Standard Standard Standard Standard QC OC QC QC QC Standard Standard Standard Standard Standard Standard Standard Standard Standard fltd Cone 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 Kt 7.080 7.094 7.093 7.083 7.079 7.106 7.104 7.095 7.107 7.105 7.105 7.106 7.106 7.084 7.105 7.103 7.104 7.107 7.105 7.104 7.107 7.101 7.106 7.100 7.099 7.105 7.117 7.083 7.105 7.106 7.102 7.098 7.106 7.103 7.097 7.083 7.107 7.105 7.08S 7.105 7.102 7.100 7.105 7.085 7.107 7.106 7.104 7.0S3 7.098 7.106 7.106 7.101 7.104 A m Flags Cone. %Pnr 1066 bb 1185 bb 1198 bb 1222 bb 1311 bb 1493 bd 1689 bb 1526 bb 1402 M4 1774 bb 1625 bb 1335 bb 1369 bb 1680 bb 1602 fab 1633 bb 1598 bb 1543 bb 1570 bb 1324 bb 1367 bb 1577 bb 1301 bb 1102 bb 1422 bb 1547 bb 1S8B bb 1497 bb 1433 bb 1329 bb 1570 bb 1160 MM 1165 bb 1142 bb 1172 bb 1254 bb 1502 tob 1318 bb 1238 bb I486 bb 1192 bb 1485 bb 1543 bb 1541 bb 1540 bb 1561 bb 1595 bb 1499 bb 1357 bb 1689 bb 1574 fab 1415 bb 1441 bb 0.70 0.78 0.79 0.81 0.87 0.99 1.12 1.01 0.93 1.17 1.08 0.88 0.91 -30 -22 -21 -19 -13 -1 12 1 -7 17 8 -12 -9 1.11 1.06 1.08 1.06 1.02 1.04 11 6 8 6 2 4 0.88 0.90 1.04 0.86 0.73 0.94 -12 -10 4 -14 -27 -6 1.02 1.05 0.99 0.95 0.88 1.04 2 5 -1 -5 -12 4 0.78 0.77 0.76 0.78 0.83 0.99 -22 -23 -24 -22 -17 -1 0.87 -13 0.82 -18 0.99 -1 0.79 0.98 1.02 1.02 1.02 1.03 1.06 0.99 0.90 1.12 1.04 0.94 0.95 -21 -2 2 2 2 3 6 -1 -10 12 4 -6 -5 K3dV a t a r g t T n l ^ l t ' 0 a 4 a n o f und. lAC to/cuhl Paga 4 BEST COPY AVAILABLE ovp 020199: Quantifiai ani ?: .tel by laa on 10/19/99 00584 ------------------------------------------------------------------------------------------------------------------- :---------------------------------------------------------------------------- __________________________ i Quantify Calibration Report fOZl9-rat aara, day l a i, control a doaa- art. 10/19/99 >S> ' I <,-!</ Vaco 1 0005S5 Quantify calibration port T0JU4S-rat sara, day 1 6 . control 6 doso- ant. 10/19/ O B aPa? 000586 Calibration Raport YOXMS-rat in, day l a , control & dosa- ant. 10/D/tt m p*gm 3 000587 Quantify Calibrati M p o r t ___ T O l U S n t i m , day 1 4 4, control A 4oa~ M t . 10/19/9# OBI V 4 9 000588 BEST COPY AVAILABLE Wechci Report Mache 1 file: Lase tc :i:ed: Cotrpc .r. Print*..! C;". 3SLY! oup-rata.pro\MethDB\101999b.*db . :ct 2: :36:4S 1999 liA {( Ot 2: i:10:55 1999 Coirpo ! Name: Incar h1 Ref.: Quant.:y Trace: Core, c f Standards: User RF Value: User Pe.nk Factor: Integrate Windcw Facttr Chrom.sttgra.'B maJ win- OAA (Chi) Nona ] .IC -ixed 1.000000, Disabled 1.000000 2.000 ..OOOODa Recenti :n Time (nir.i': Relat" - ?scantier. RT Re. Time ;:v (mini' Peak _'c'.action: -.133. Enabled .000, Disabled None] .334 earest Respo- -r Type: Rerpe .. External \reas Polyntir lal Type: Point c: Origin: Pit W-l jhcir.c: Axis 7.-insfermacion: linear -xcluds 1/X :or.e Units: Peak- amp'..' .. ? Smce t Wir.dc v -iz* (scir.j . Wur.be. SlRCOt g method: nabled Join . .ley threshold; Reduc eak tailing: Raise - -- maximum.: 0.00 :o.oo .:o Draw Detec Shcul 't 'relhcld: :.oo disabled 10.00 Relit - 3ht : AbsC. Relat. - .;3: Afcscl : *..=J: .50, Diaabled .00, Disabled :.00, Diaabled .00, Oisabled ' . A . ____~ / ! .f4 Page 1 >?o/ff 7 1 ms 000589  C I u u r r M V M IL M D L .C Me: h c . l ?ep:rt Me:h e i iile: La:t -o Lfiad: Cor pe .nJ Printed: C:\XASSLYT :up-raes.pro\MethD>\101999b.adb Wed Oce 2C :36:4t 1999 2: PP0S <C v.'ed Oct 2: 7:10:55 1999 Ccn .r. r-ir: In:4: .i. h f.: Quer.: t-. T r a c e : Os*r ?.? .`a'.je: Ose r re . - a c t o r : Xntaer.^-.* Vtr.dcw Tac: Chzar^::i-r OS (Ch2 > :onel . :c sne. B ..000000, Disabled 1.000000 .000 ..00000a Re* er -1: Tirre '.z.Lr.z Re: s: -- 7.:.-i: RT Re t.-.r.;e; Tire ' . :v (~lr =:. Pef7< Se l e c t i o n : .3G6, Bnablad .OSO, Disabled :;onej .411 arast RejV'-**T T'.'pe : Rei : cernal ress Pol vr.:ir.ia1 7Y?* : Po:*:: c; Crtin: Pi: 'M-.l,:hti::i: Axij 7r -r.3: :i:r.r -inear xclude ./X ': n e Sir.-:et-.in;:- W ird: j .z* U r in s ' : u . r - 4 c : ,=:nc : : : Srr:-* .: ::et:-.: Je.: : 1: ::.r- :Id: Re. :r; = Ra:.* D n - 4 . : . : . : * re. :1 De:*:: Sh: -1 :..reir.;l: R e : -: : . R e a : . . ? : rea At : 1 (;: rnabled :.o o :z .00 .00 ..00 taabled 0.00 -SO. Disabled .00, Disabled ..00. Disabled .00. Disabled S t ozvirt f X ke Pape 2 B E ST C O P Y AVAILABLE 000590 BEST COPY AVAILABLE Me- ;; r: '.XASSLY: L*. '. .1........ i Cct 2. Cc:: i: ?FCSA `..t : Ccr 2( ou;-race.pro\XeehDB\101999b.adb :3:4t 1999 ) 10:S` l M 9 Ccr - v .r . J r-r.e: i n - :-.i. : Q u t r . i : / " i-iCr: Ccr c f iris: ?rOSA (ChJ) NOO#) rtc :onc. C D*i r -F V ** - In- Ch: ..>i '- ~v t : ..s --.aw: 000000. Disabled oooooo :.o o o .OOOODa Re- '' . ` r e r-.r. Re : - izr. T i - e . RT i.:.. Ti:r . . . . . . i-i-s' : h f - .= ec ;ior.: '.SS7, Enabled .0C0, Oisablad .Nor.*] .735 earat Res-v.se r-.-ceRes I t : :xteraal reas Pc:/r. mis'. Fi*. -.V r Ax: . .'ri-.. ..;v:lirv linear 'xclude /X Zona Bn: r.* Fts. '-.I- : 3 Sff-. Mir Hu.* Sr: i .: i (-nr.i. : :f z:r.oc\: 5 r.abled Re - - . -v: Rr..- .:..r.ua: .3.00 .30.00 .00 Or- - . c'.i *0.00 De disabled Sh- . 0.00 Re ' At.' . Re: :Z . . Abi-1 ,:4: ..ed: .S3, Oiaablad .00. Disabled .00. Disabled .30. Disabled * oia if? JJtS Fi9* 3 000591 b t O I U U K Y A V A IL A B L b M* t h ' - ; U . : nc-. .*d: Ccr : : in 1 P r i ; : -d: C: \XASSLY: *oup>raes.pro\MethDB\101999b.adb Wed C e t 2! '.36:41 1999 4: IS (Chi wed C c t 2C -:10:S6 1999 Cor : .r. ! *' ,;-'9 : I n ; : -a '. . Qur . f .- : Cor.-, c : J ir.dards : W st- RF \`a Lue : Ust - >c t a r : I r ; ' : - 1Tv F a c to r : C h .i^ T f. . . .... t iS window; : s (Ch4) 'Non*) -ic .-'ix*d 1.000000, D isabled ..000000 1.000 : . oooooa Re- ; Re ! - . RT Ti-" Per -.S..r . . Tiv.e : .- ; - i c r. : 1.152, Enabled .000, Disabled Nona] '.323 .rest R e ! T' Res. i ..-a: External \raas P o .. .i:.T.isl Type: P o : ..: c : ' ' ; 7 ; r. : P ir W e-ci.; : rvy : A:: T r f - i e r t i : i : n : lin e a r Exclude i/X iene Or., u: Pc - ; L. :u d e : 9 Sr. : Wir I. ; Ml* . , . Src - 1s : \ r.s ' : -is : : .e:`:od: -'cabled J c ;.. threshold: Ree z %. : c 5i 1 i r. j : R* '-i : ... Dl : V -r . De- r- s SI ... r -, - ....... - ^ . :J: R Al Re Ai. . ... .. .J. -.3 : 0.00 00.00 .00 0.00 disabled 10.00 1.50. Disabled .00, Disabled 1.00, Disabled .00. Disabled * l* i 1 tag 4 000592 Q uattro II, #6414E ' SOUP 020199: FACT Equipment Log 99092 PAGE 1/1 DATE: 10/19/99 ANALYST:mmh STUDY NUMBER: TOX145 MATRIX: rat sera DESCRIPTION:Davs 1.4 FACT Method: ETS-8-5.1 Injection volume: 10 uL __ Cycle time: 10 min. Electrode: ZiStm y______ Mobile Phase: (A12.0 mM NH4CH3C02 (B).MQH_____ TN-A- or stndrd number (A) 99085-10-14 (B) TN-A-2997 Prepared (date/by): (A 110/16/99 mmh_______ (B) m O S l a b Expires: (A) 04/00______________ (B)_2.Q1Q______ Store at room temp? @ or N Other:. G uard column: None__________________ Part number: na_________ Lot number: na Analytical column: Keystone Betasil___________________________________ Size: 2 x 50 mm________________ Type: C18___________ Sphere size: 5 urn Part number: 055-701-2__________ Lot number: P9E11 Serial number:05918042 Analytical parameters: Drying gas (TVhr'l: 350 ESI nebulizing gas (L/hrl 13 LC Flow rate: 300 uL/min. Back pressure: 65 bar Sheath gas (I7hr)_Q. HPLC solvent gradient: 10min-10-95 Time (min,)____ DJLQfl_______ 2LLQ_______ 3 L L 5 Q _____________ _____ 51LQQ________ %B JM JM 91a 212. 1M L 0C0593 BEST COPY AVAILABLE Timing Method Report Method: C:\MASSLYNX\S0UP-RATS.PR0\ACQUDB\PP0S3 Printed: Tue Oct 19 15:40:03 1999 / W # Page 1 MS SOURCE { ESP- ) CapillaryCone Extractor RF Lens Source Block Temp. Desolvation Temp. MS2 Set Rdbk 3.00 40 5 0.2 150 250 3.01 -41 -8 150 251 Pressures Analyser Vacuum Gas Cell Rdbk 5.5e-5 4.le-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set 14.0 14.0 0.9 0.0 4 650 Set Rdl 14.0 14.0 10 2.0 0.0 40 0 650 8 38 1 000594 Method: c iVM*MLna\*oor-iut*t.paovucguDSN1OKM-pFoa-poah-PFasa-xs. L u t Modici*: tri Oct IS 11*)S:03 1 > M Print*: Tu* Oct It 15:40:3 1 Solvent Delay ( Mina ) : 0.00 Function : 1 MtM of 1 Maas Fair ( ESP- ) Inter Channel Delay { Seca ) : Span ( Deltona ) : Start Tiae ( Nina ) : Snd Tiae < Mina > : Repeat* : Channel Parent Daughter 0.01 0.00 0.00 10.00 1 Dwell (Seca) Coll energy (eV) Cone ( V ) 1 413.00 169.00 0.30 30 IS Function i 3 MRM of 1 Mas* Fair ( ESP- ) Inter Channel Delay ( Secs ) : Span ( Dalton* ) : Start Tiae ( Mina ) : Snd Tina ( Min* ) : Repeata : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) Coll Snergy (*V) Cone ( v 1 499.00 99.00 0.30 45 <0 Puaotlon : 3 N M of 1 Mass Fair < SSP- > Inter Channel Delay i[ Seca ) : Span ( Daltona ) : Start Tiae ( Mina ) i Snd Tiae ( Mina ) : Repeata : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) Coll Snargy (av) Con* 1I v 1 498.00 78.00 0.30 45 60 Function : 4 MRM of 1 Masa Fair { ESP- > Inter Channel Delay I: Secs ) : Span ( Daltons ) : Start Tiae ( Mins ) : Snd Tisw ( Mina ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) Coll Energy <eV) Cone i: v 1 427.00 80.00 0.30 40 60 000595 Masslynx - Sample List Sample List: C:\MASSLYNX\soup-rats.pro\SampleDBW01999b.SPL' Printed: Tue Oct 19 15:42:35 1999 Page 1 P age Position: (1 ,1 ) File Name File Text MS R ie 1 101999012 M eO H Blank 2 101999013 M eO H Blank 10M IN -P FO S -P O A A -P FO S A -IS 10M IN-PFOS-POAA-PFOSA-IS 3 101999014 M e O H Blank 10M IN-PFOS-POAA-PFOSA-IS 4 101999015 TO X145-R B S 1019 9 -H 2 0 Blank-11, SEE 10M IN-PFOS-POAA-PFOSA-IS 5 101999016 TO X145-R B S10199-Sera Blank-11, SEE 10M IN -P FO S -P O A A -P FO S A -IS 6 101999017 TO X145-R TS10 1 99-Sera Blank-11, SEE 10M IN -P FO S -P O A A -P FO S A -IS 7 101999018 TO X145-R TS10 1 99-Sera Blank-12, SEE 1O M IN -P F O S -P O A A -P F O S A -IS 8 101999019 T O X 1 45-R B S 10 1 99-5p pb-11, SEE 10M IN-PFOS-POAA-PFOSA-IS 9 101999020 T O X 1 45-R B S 10199-10p pb -11, S E E 10M IN-PFOS-POAA-PFOSA-IS 10 101999021 TO X145-RBS10199-25ppb-11, SEE 10M IN-PFOS-POAA-PFOSA-IS 11 101999022 TO X 145-R B S 10199-50p pb -11, S E E 10M IN-PFOS-POAA-PFOSA-IS 12 101999023 TOX145-RBS10199-100ppb-11, SEE 10M IN-PFOS-POAA-PFOSA-IS 13 101999024 T O X 1 45-R B S 10 1 99-250pp b-11, S EE 10M IN-PFOS-POAA-PFOSA-IS 14 101999025 T O X 1 45-R B S 101 99-500 p p b -11, S EE 10M IN-PFOS-POAA-PFOSA-IS 15 101999026 TO X 145-R B S 101 99-750 p p b -11, S EE 10M IN -P FO S -P O A A -P FO S A -IS 16 101999027 T O X 14 5 -R B S 10199-1000ppb-11, S E E 10M IN-PFOS-POAA-PFOSA-IS 17 101999028 M eO H Blank 10M IN-PFOS-POAA-PFOSA-IS 18 101999029 TO X145-R TS, 9R 03230M , D y l, Control,-10(19/99 SEE 10M IN-PFO S-PO AA-PFO SA-IS 19 101999030 TO X 145-R T S , 9R 03231M , D y l, Control,-10/19/99 SEE 10M IN-PFO S-PO AA-PFO SA-IS 20 101999031 TO X145-R TS, 9R 03232M , D y l, Control,-10/19/99 SEE 10M IN-PFO S-PO AA-PFO SA-IS 21 101999032 T O X 1 45-R T S , 9R 03 233 M , D y l, Control,-10/19/99 SEE 10M IN -P FO S -P O A A -P FO S A -IS 22 101999033 TO X145-R TS, 9R03234M , Dy1, Control,-10/19/99 SEE 10M IN-PFO S-PO AA-PFO SA-IS 23 101999034 TO X145-RBS10199-250ppb-CCV-11-1, SEE 10M IN-PFOS-POAA-PFOSA-IS 24 101999035 M e O H Blank 10M IN-PFOS-POAA-PFOSA-IS 25 101999036 TO X145-R TS, 9R 03235M , Dy4, Control,-10/19/99 SEE 1OMIN-PFOS-POAA-PFOSA-IS 26 101999037 TO X145-R TS, 9R 03236M , Dy4, Control,-10/19/99 SEE 10M IN-PFO S-PO AA-PFO SA-IS 27 101999038 TO X145-R TS, 9R 03237M , Dy4, Control,-10/19/99 SEE 10M IN-PFO S-PO AA-PFO SA-IS 28 101999039 TO X145-R TS, 9R 03238M , Dy4, Control,-10/19/99 SEE 10M IN-PFO S-PO AA-PFO SA-IS 29 101999040 TO X145-R TS, 9R 03239M , Dy4, Control,-10/19/99 SEE 1OMIN-PFOS-POAA-PFOSA-IS 30 101999041 T O X 1 45-R B S 10199 -250pp b-C C V -11-2, SEE 10M IN-PFOS-POAA-PFOSA-IS 31 101999042 M eO H Blank 1O M IN -P F O S -P O A A -P F O S A -IS 32 101999043 T O X 14 5 -R T S 1 0 1 99-250pp b-M S -11 ,1 0 /1 9 /9 9 SEE 10M IN-PFOS-POAA-PFOSA-IS 33 101999044 TO X145-R TS10199-250ppb-M SD -11,10/19/99 SEE 1 0 M IN -P F O S -P O A A -P F O S A -IS 34 101999045 T O X 1 45-R T S , 9R 03245M , D y l, 5 m g/kg 10/19/99 SEE 10M IN -P FO S -P O A A -P FO S A -IS 35 101999046 T O X 1 45-R T S , 9R 03246M , Dy1, 5 m g/kg 10/19/99 SEE 1O M IN -PFO S -P O A A -P FO S A -IS 36 101999047 T O X 1 45-R T S , 9R 03247M , D y l, 5 m g/kg 10/19/99 SEE 10M IN -P FO S -P O A A -P FO S A -IS 37 101999048 TO X145-RBS10199-250ppb-CCV-11-3, SEE 10M IN -P FO S -P O A A -P FO S A -IS 38 101999049 M eO H Blank 10M IN -P FO S -P O A A -P FO S A -IS 39 101999050 T O X 1 4 5 -R T S , 9R 03 248 M , Dy1, 5 mg/kg 10/19/99 SEE 10M IN -P FO S -P O A A -P FO S A -IS 40 101999051 TO X145-R TS, 9R 03249M , D y l, 5 mg/kg 10/19/99 SEE 10M IN-PFOS-POAA-PFOSA-IS 41 101999052 T O X 1 4 5 -R T S , 9R 03250M , Dy4, 5 m g/kg 10/19/99 SEE 10M IN -P FO S -P O A A -P FO S A -IS 42 101999053 TO X145-R TS, 9R 03251M , Dy4, 5 mg/kg 10/19/99 SEE 10M IN-PFOS-POAA-PFOSA-IS 43 101999054 TO X145-R TS, 9R 03252M , Dy4, 5 mg/kg 10/19/99 SEE 10M IN-PFOS-POAA-PFOSA-IS 44 101999055 TO X145-RBS10199-250ppb-CCV-11-4, SEE 10M IN -P F O S -P O A A -P F O S A -IS 45 101999056 M eO H Blank 10M IN -P F O S -P O A A -P F O S A -IS 46 101999057 TO X145-R TS, 9R 03254-1M , Dy4, 5 mg/kg 10/19/99 SEE 10M IN-PFOS-POAA-PFOSA-IS 47 101999058 TO X145-R TS, 9R03254-2M , D y 4 ,5 mg/kg 10/19/99 SEE 10M IN-PFO S-PO AA-PFO SA-IS 48 101999059 TO X145-RBS10199-250ppb-CCV-11-1, SEE 10M IN-PFOS-POAA-PFOSA-IS 49 101999060 M eO H Blank 50 101999061 TO X145-R B S 10199-H 2O Blank-11, SEE 51 101999062 TO X 1 45-R B S 101 99-S e ra Blank-11, SEE 10M IN-PFOS-POAA-PFOSA-IS 10M IN-PFOS-POAA-PFOSA-IS 10M IN-PFOS-POAA-PFOSA-IS 52 101999063 TO X145-R TS10199-Sera Blank-11, SEE 53 101999064 TO X145-R TS10199-Sera Blank-12, SEE 54 101999065 TOX145-RBS10199-5ppb-11, SEE 55 101999066 TOX145-RBS10199-10ppb-11, SEE 56 101999067 TOX145-RBS10199-25ppb-11, SEE 57 101999068 TOX145-RBS10199-50ppb-11, SEE 58 101999069 TO X 145-R B S 101 99-100 p p b -11, S E E 59 101999070 T O X 1 45-R B S 10199 -250 p p b -11, SEE 10M IN -P FO S -P O A A -P FO S A -1S 10M IN-PFO S-PO AA-PFO SA-IS 10M IN-PFO S-PO AA-PFO SA-IS 10M IN-PFO S-PO AA-PFO SA-IS 10M IN-PFO S-PO AA-PFO SA-IS 10M IN-PFOS-POAA-PFOSA-IS 10M IN-PFOS-POAA-PFOSA-IS 10M IN-PFOS-POAA-PFOSA-IS 000596 Masslynx - Sample List Sample List: C:\MASSLYNX\soup-rats.pro\SampleDB\101999b.SPL: Printed: Tue Oct 19 15:42:35 1999 Inlet File Bottle Inject Volume Sample Type Cone A 1 10nnin-10-95 91 2 10m in-10-95 91 3 10m in-10-95 91 4 10min-10-95 1 5 10min-10-95 2 6 10min-10-95 3 7 10min-10-95 4 8 10min-10-95 5 9 10min-10-95 6 10 10min-10-95 7 11 10m in-10-95 8 12 10min-10-95 9 13 10min-10-95 10 14 10m in-10-95 11 15 10min-10-95 12 16 10min-10-95 13 17 10min-10-95 92 18 10min-10-95 14 19 10m in-10-95 15 20 10min-10-95 16 21 10m in-10-95 17 22 10min-1O-95 18 23 10m in-10-95 41 24 10min-10-95 92 25 10m in-10-95 19 26 10min-10-95 20 27 10m in-10-95 21 28 10min-10-95 22 29 10min-10-95 23 30 10min-10-95 42 31 10m in-10-95 92 32 10min-10-95 24 33 10min-1Q-95 25 34 10min-10-95 26 35 10min-10-95 27 36 10min-10-95 28 37 10min-10-95 43 38 10min-10-95 93 39 10min-10-95 29 40 10min-10-95 30 41 10m in-10-95 31 42 10min-10-95 32 43 10min-10-95 33 44 10min-10-95 44 45 10min-10-95 93 46 10min-10-95 34 47 IOmin-10-95 35 48 10m in-10-95 41 49 10min-10-95 93 50 10min-10-95 1 51 10m in-10-95 2 52 10min-10-95 3 53 10min-10-95 4 54 10min-10-95 5 55 10min-10-95 6 56 10min-10-95 7 57 10m in-10-95 8 58 10min-10-95 9 59 10min-10-95 10 10 .... 10 10 ... _ 10 -- 10 ... 10 10 10 -- 10 ... 10 10 _ 10 ... 10 -- 10 __ 10 10 10 -- _ _ 10 10 __ _ 10 10 _ 10 -- 10 __ 10 -- 10 -- 10 __ 10 __ 10 __ 10 __ 10 __ 10 __ 10 10 ... 10 ... 10 __ 10 ... 10 __ 10 __ 10 __ 10 __ 10 __ 10 ... 10 __ 10 10 10 10 __ 10 __ 10 __ 10 __ 10 __ 10 __ 10 __ 10 __ 10 __ 10 ... 10 ... 10 10 -- --- _ -- -M. -- ... -- Page 2 Page Position- (2 1) 000597 Masslynx - Sample List Sample List: C:\MASSLYNX\soup-rats.pro\SampleDB\101999b.SPL' Printed: Tue Oct 19 15:42:35 1999 File Name File Text 60 101999071 TO X 1 45-R B S 10199-500pp b-11, SEE 61 101999072 TO X 1 45-R B S 10199-750pp b-11, SEE 62 101999073 TOX145-RBS10199-1000ppb-11, SEE /dl Page 3 Page Position: (1 2) MS File 10M IN -P F O S -P O A A -P F O S A -IS 1O M IN -PFO S-PO A A -PFO SA -IS 1O M IN -P F O S -P O A A -P F O S A -IS 000598 Masslynx - Sample List Sample List: C:\MASSLYNX\soup-rats.pro\SampleDBYI01999b.SPL! Printed: Tue Oct 19 15:42:35 1999 Inlet File Bottle Inject Volume Sample Type Cone A 60 10m in-10-95 11 61 10m in-10-95 12 62 10m in-10-95 13 10 10 10 Page 4 P age Position: (2, 2) 00S 99 FACT: DATA REVIEW SUM M ARY FO RM Date: Data Analyst 3S Dats Review Sign-Off Analyst Review Name / Date: :, IAC FACT Study #: To* M 4 Matrix/Timepoints: T Z j- tro . 'D t/u Jr cS - ^ a j * Technical Review . Name/Date: /to? / o / ? r / W Sample hZ*t1< L Set-up Analysis Date/Analyst: Instrument AkJLi O M f ! Analyte: ~fO& 6 # l ) J LAcceptable Linear Range: L O Q : ___ A ____________________ RA2: A4-______________ Extraction Blank VA A/Matrix Blank a Calibration Checks: A________ MS/MSD: K in ) tnUrtA Data Status: __ pa)- Analvte: TfcoS Cc/t*}<> Quality Assurance Review Name / Date:_____________ Data Entry: AW e n lW tlU L y + ^d u -u IC .............. " ^ Comments/Justifications: ________________________ <>% MS >L> Cuvu*. su. t4 L -/Ca S * ~ j.L sd ~ J* r foA , /s u sclfj -Per A na, n*J s <UeJ Vt-b-bK -b**S kJ skc. <f<oC x L j J /L a -/ b . llS * J .____ p u i s & e t u J - b ___ k * r S M /*- tt* - Toas , c+m l / . 4%*-c* U I tU X S & jJ * / ____ -- T * s l * f z s - h y r/Ls Jtr ^s_______ Acceptable Linear Range: -23 rL 4ajL J 4 4 o S u x J * c A t{ -4-eJ~ LQ :___iTt.7e3rhi RA2: O .ftS Extracted Blank / x tQ Matrix Blank &*.*. U)Q lK lc4/os -foLj e j -fa y- C o -fel*/-L.< rfu-c - i &c4- <d~ s tu x jL . 74a. Calibration Checks: t J J f PLjJ> *y v c j o t K . A* MS/MSD:____r L f l A Q ^ l L ____________________L A l Data Status:____________V__________________________ ___ t f o n d 4 * "pYiJtde. O ^ J a o j / sk 44 4a 4La. <**</ 4* Analyte: TSA Acceptable Linear Range: LOQ:___ ffL , Extracted Blank: f a s 7**a-GI RA2: 0 f f V 5 l > Matrix Blank Jes* LO. Calibration Checksi: M S / M S D : ____ O u d I - U rta /1 / l Data Satus: u l i p / j 'f / q ? ) i m , r C u r v e g a r n i s 4 S o "/ * or- t * * * Jttn&j-toi*-._44 Atas 4*__ <hj> ~fx~ !oux.r boi-J* S 4 L 4 'H -e fa d 'iu bigjJ c L M tu - t* * 4l **-- 4a LoQ . [JCt*-* a u 4 'll* - faieit.fi' U J t4 3*7o r K -e. h l/to JA.S CMJrOt- y fit.v' t e i l e t m ^ l t 6 <5i`S 7 ' 2 e + Z & n > * j > ~ < - toe & & < : * . /Tt/JLi<4& 77*=^i f 7 7 * tr /S c ? > r 0/3* S '/ ? 9 , 0 X UiulcL Xugi^tjl- rttincl^tie^. ia m f U a Woc^ i- U-liVa / r iA pci .^ o l ' Ji d Cu r r e tr ^n, Coti)vuA>g Clitr-lkK v t n fi'c r;4>r>r. A b o . +|i\a, >-t CCt/v t 4 r t t t k A ia^-K Vht/c. O n i A i COtnn dd ^j iui . |kt>r 4 o b n c J t A v g Cufie 4o W n l v j C d 0 6 000600 FACT: DATA REVIEW SUMMARY FORM Date: Data Analyst' FACT Study#: jx /H 'TotCfc______________________________________ Matrix/Timepoints: & /, * 'P tU tju s , ^ f 4 f Sample List /^ 7 ? g _ ^ Set-up Analysis Date/Analyst y. /y n s/ff it* Instrument r>L Analvte: C c H if Acceotable Linear Ranae: HA LOO: AAa Extinction Blank: A /A R"2: AM Matrix Blank: aM Calibration Checks: MS/MSD: AJA ------- Data Status: '" Data ReviewSign-Off Analyst Review . Name / Date: ' * s lAC' Technical Review ~ . nName / Date: fi^ X ir To Quality Assurance Review Name / Date:_____________ j . i-a Data Entry:: _M . -rbrtA : nud 4o rctuolj -u. me Comments / JustUIcations: ____________________ 'o/js/t OP tiilurpedcg - t o n s , :e*5 fS z sL,u4j ht. Q -------- djJed. ClVUt. i * M ___ ipcrc- J r * f + * d - A ____________ J * L o a J fr n u u P a M H L J r /~ - A -H a . 1/ S m ijb S e d - "%* C d c l u c k s J> r b o Jo lj d w i. t4 /a d tj- . db 7F$a cb*LJ <lkJ sL * J / b miMidjdcJ ''*** r/*sU1_________________ 3 5 Srea. f a a k u ^ PrtlS&lctiJ' Jh, 4 u C ir y e s t . --p J 'L h * * b t y t k J d*jh S ^ k 2 & s t , L J J u r -tL S , >aU sU 9 M io S *~ fL s s b u fd b ff e v * * y - , t < t' due 4* /a. d b L d CeJ ejucJLc- TZe S&~+bs re lr * c b -L d L tj 4b- CttMres. 'X*. *(3) td cL tc_____ dfJiaJia/i4 Pty* ' U p h e l d d o u e ^ e y e s feat*. lee4 * / S&u^oU. b d A6________ dsCL?tt C>yu* h> l o * j 4 . X*s rfis/fl 000601 Quantify Cenpound Buneery Report TOX14S-rat eerue dilutions, day 1 ( (- oat. 10/19/9* SEE Sasplo List: C :\ASSLYKX\aaeUa-ratc.90\Sa^loO\102299a Last codified: Han Oct 29 06:43:9 19*9 Method: C:\Mk6SLTNX\MMlla-rato. MO\MsthOS\102299a Last oodiflod: Mon Oct 29 06:39:99 1999 Job Code: Printed: ton Oct 29 06:99:42 19*9 Ceepound 1: POAA <Chl) Mane 1 102299001 2 102299002 3 102299003 4 102299004 5 102299005 6 102299006 7 102299007 6 102299009 9 102299009 10 102299010 11 102299011 12 102299012 13 102299013 14 102299014 19 102299015 16 102299016 17 102299017 18 102299019 19 102299019 20 102299020 21 102299021 22 102299022 23 102299023 24 102299024 25 102299025 26 102299026 27 102299027 28 102299028 29 102299029 30 102299030 31 102299031 32 102299032 33 102299033 34 102299034 35 102299035 36 102299036 37 102299037 38 102299038 39 102299039 40 102299040 41 102299041 Sasplallst Test Type MeOH Blank MeOM Blank TCX145-RBS1Q199-H20 Blk-12, SEE TQX145-RB310199-S*nas Blk-12, SEE TOX14S-RTS10199-Serue Blk-12, SEE TOX145-RBS1019*-Spp-12, SEC TQX14S-RBS10199-10ppb-12, SEE TQX14S-*BS1019-25ppb-2, SEE TOX14S-RBS10199-SOppfer-12, SEE Standard Standard Standard Standard T0X14S-RBS10199-100ppb-12, SEE Standard TOX145-RSS10199-2SOppb-12, SEE T0X145-RBS10199-S00ppb-12, SEE T0X145-RBS10199-7S0pjpb-12, 5EE TOX145-RB51O19B-10OOppb-12, SEE Standard Standard Standard Standard MeOH Blank TCK145-RTS-9R0324SM, Dayl, 5eg/kg, DSO-axtlO/19/99 TC0U45-RTS-9RO3246M, Dayl, Sag/kg, DSO-axtlO/19/99 TCDC145-RTS-9R03247M, Dayl, Seg/kg, D50-extlO/19/99 7OX145-RTS-9R03246K, Dsyl, 5eg/kg, D50-sxtl0/19/99 TOX14S-RTS-9R03249K, Dayl, 5eg/kg, D50-exel0/19/99 70X14S-RBS1019B-2S0ppb-CCV-11-1, SEE QC MeOH Blank TOX145-RTS-9R032SOM, Day4, 5eg/kg, D50-sxtl0/19/99 TOX145-R7S-9R03251M, Day4, 5ag/kg, DSO-axtlO/19/99 TOX145-RTS-9R03252M, Day4, 5eg/kg, DSO-sxtlO/19/99 7QX145-R7S-9R03254-1M, Day4, Seg/kg, DS0- 10/19/99 TOX145-R7S-9R03254-2M, Day4, Sag/kg, 050- 10/19/99 TOX14S-RBS10199-2SOppb-CCV-11-2, SEE QC MsOH Blank TOX145-RBS10199-K20 Blk-12, SEE T0X145-RBS10199-Serue Blk-12, SEE TOX145-R7S10199-Serue Blk-12, SEE 70X14S-RBS10199-5ppb-12, SEE Standard TOX145-RBS10199-10ppb-12, SEE TOX145-RBS10199-25ppb-12, SEE Standard Standard 70X145-RBS10199-50ppb-12, SEE TGX145-RBSl0199-1OOppb-12, SEE Standard Standard TOX145-RBS10199-250ppb-12, SEE TOX145-RBS10199-SOOppb-12, SEE TOX145-RBS10199-750ppb-12, SEE TOX145-RBS10199-1000ppb-12, SEE Standard Standard Standard Standard SCd 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 1.00 1.00 1.00 1.00 1.00 1.00 1.00 RT 6.990 6.997 7.015 7.000 7.027 7.010 6.998 6.989 6.995 6.998 6.996 7.006 6.997 6.974 6.994 6.995 6.965 6.996 7.018 7.000 6.972 6.992 6.997 7.094 6.993 6.999 6.990 6.996 7.001 7.022 6.996 7.001 7.016 6.998 6.997 6.980 '3 * a SL-bjJ Rapo 1 Area Cono. flag tDev 120 1.04 bd 4 109 0.94 bb -6 115 0.99 m -1 110 0.95 bb -5 125 1.08 bb 6 110 0.95 bb -5 97 0.84 db -16 75 0.65 bb -35 118 1.02 bb 2 142 1.22 bb It 76 0.66 bb -34 158 1.37 bb 37 24 0.21 bb -79 34 0.29 bb -71 36 0.31 bb -69 29 0.25 bb -75 26 0.23 bb -77 77 0.66 bb -34 20 0.17 db -63 25 0.21 bb -79 26 0.23 bb -77 22 0.19 bb -91 52 0.45 bb -55 11 0.10 bb -90 117 1.01 bb 1 119 1.03 bb 3 94 0.81 bb -19 105 0.91 bb -9 136 1.19 bd 19 117 1.01 bb 1 104 0.90 bd -10 73 0.63 db -37 138 1.19 bb 19 160 1.38 bb 38 95 0.82 bb -18 143 1.24 bb 24 Am U i 062496: Quantitated and Printed by iaa 10/29/99 000602 Quantify C a ^ o u n d l i a B u y teport TOXl4S-rat u n a dilution, day 1 H - at. 10/19/99 9SS Staple Lit: C: \MABSUrMX\amelle-imt .PK>\SaapleDB\X02299a Laat modified: Hon oet 29 09:43:99 1999 Method: C:\MASBLTWC\amelie-rata.PRO\MethDB\102299e Last aodifiad: Mon Oet 29 09:39:99 199 Job Coda: Printed: Mon Oet 25 09:99:42 1999 Compound 2: PFOS (0x2) 9 Maae 1 102299001 2 102299002 3 102299003 4 102299004 5 10229900S 6 102299006 7 102299007 9 102299008 9 102299009 10 102299010 11 102299011 12 102299012 13 102299013 14 102299014 15 102299015 16 102299016 17 102299017 18 102299018 19 102299019 20 102299020 21 102299021 22 102299022 23 102299023 24 102299024 25 102299025 26 102299026 27 102299027 28 102299028 29 102299029 30 102299030 31 102299031 32 102299032 33 102299033 34 102299034 35 102299035 36 102299036 37 102299037 3B 102299038 39 10229903 40 102299040 41 102299041 Sanpleliat Text Type MeOH Blank Medi Blank TOX14S-ABS10199-H2O Blk-12, SEE TOX14S-ABS10199-Serom Blk-12, SEE TOXl45-AT510199-Serum Blk-12, SEE TOX145-ABS10199-5ppb-12, SEE Standard T0X145-RBS10199-10ppb-12, SEE Standard T0X145-M510199-25ppb-12, SEE Standard TOX14S-R8S10199-50ppb~12, SEE Standard TOX145-RBS10199-100ppb-12, SEE Standard TOXl45-RBS10199-250ppb-12, SEE Standard TOXI45-R8510199-500ppb-12, SEE Standard TOXl45-RBS10l99-750ppb-12, SEE Standard TOX145-ABSl0199-1000ppb-12, SEE Standard Medi Blank TOX145-ATS-9B03245M, Oayl, 5mg/kg, 05Q-e*t20/19/9 TOX14S-RTS-9A03246M, Dayl, 5mg/kg, 050-extl0/19/99 TOX145-ATS-9R03247K, Dayl, Smg/kg, DS0-extl0/19/99 TOX14S-ATS-9A03248M, Dayl, Smg/kg, DSO-extlO/19/9t TOX14S-RTS-9R03249M, Dayl, Smg/kg, OSO-extlO/19/99 TOXI45-RBS10199-250ppb-CCV-11-1, SEE QC MeOH Blank TQX145-RTS-9R0J250H, Day4, Smq/kq, D50-extl0/19/99 TOX145-RTS-9R03251M, Day4, 5mg/kg, D50-extl0/19/99 TOX145-RTS-9R03252M, Day4, Smq/kq, D50-extl0/19/99 TOX145-RTS-9R03254-1M, Day4. 5mg/kg, DS0- 10/19/99 TOX145-RTS-9R032S4-2M, Day4, 5mg/kg, DS0- 10/19/99 TOX145-ABS10199-250ppb-CCV-l1-2, SEE QC MeOH Blank TOXl45-RBS10199-H2O Blk-12, SEE TOX14S-RBS10199-Serua Blk-12, SEE TOXl45-RTS10199-Serum Blk-12, SEE TOXl45-RBS10199-Sppb-12, SEE Standard TOX145-RBS10199-10ppb-12, SEE Standard TOX145-RBS10l99-25ppb-12, SEE Standard TOX145-RBS10199-50ppb-12, SEE Standard TOX14S-AB510199-100ppb-12, SEE Standard TOXl45-RBS10199-250ppb-12, SEE Standard TOXl45-RBS10199-500ppb-12, SEE Standard TOK145-RB510199-750ppb-12, SEE Standard TOX145-RBS10199-1000ppb-12, SEE Standard Btd Cone 4.93 9.76 24.80 49.30 97.60 248.00 493.00 735.00 976.00 248.00 248.00 4.93 9.76 24.80 49.30 97.60 248.00 493.00 735.00 976.00 M 7.190 7.183 7.186 7.170 7.162 7.171 7.176 7.184 7.173 7.164 7.166 7.169 7.169 7.179 7.172 7.169 7.173 7.143 7.168 7.161 7.168 7.165 7.168 7.172 7.168 7.164 7.169 7.170 7.171 7.165 7.172 7.163 7.169 7.173 7.194 7.169 7.173 7.189 7.171 7.169 7.175 Area 119 82 112 88 263 330 528 1195 1909 5512 11228 22030 28219 36823 109 4125 6459 5637 3710 4380 168 40 4350 4238 6453 5257 4193 217 23 75 96 262 336 521 1235 2005 S514 11233 21189 29094 37681 Cone. Plage %Dev 0.24 MM 0.00 KM 0.08 MM 0.00 MM 3.44 bb 4.94 bb 0 9.34 bb -4 24.22 bb -2 40.12 bd -19 120.40 bb 23 247.73 bb -0 488.41 bb -1 626.31 bbx -15 818.00 bbX -16 0.01 m 89.49 bb 141.49 bb 123.18 bb 80.23 bb 95.16 bb 1.33 bb -99 0.00 MM 94.50 bb 92.01 bb 141.35 bb 114.70 bb 91.01 bb 2.42 bb -99 0.00 MM 0.00 MH 0.00 MM 3.43 bb 5.07 bb 3 9.20 bb -6 25.11 bb 1 42.26 bb -14 120.43 bb 23 247.86 bb -0 469.68 bb -5 645.81 bbx -12 837.11 bbx -14 2 Aaalia 092499: Quantitated and Printed by lea 10/25/99 000603 Quantify Co t mind Sunaary Raport TOXJ45-rat M r u a dilutions, day 1 S 4- nxt. 10/19/ S U S a r i * U l t : C :\MRSSLTHX\nulia-rata.PK>\SaTloO\10229a Last aodifiad: Mon Oet 25 0C:I3:S( 190 Hathod: C:\MkSSLTMX\aaalla-rat.VH0\Mathoa\102299a Last aodifiad: Mon Oet 25 0C:39:SS 1999 Job Coda: Printad: Hon Oct 25 05:59:42 199 Coopound 3: POSA <Ch4> Nana 1 102299001 2 102299002 3 102299003 4 102299004 5 102299005 6 102299006 7 102299007 8 102299008 9 102299009 10 102299010 11 102299011 12 102299012 13 102299013 M 102299014 IS 102299015 16 102299016 n 102299017 18 102299018 19 102299019 20 102299020 21 102299021 22 102299022 23 102299023 24 102299024 25 102299025 26 102299026 27 102299027 28 102299028 29 102299029 30 102299030 31 102299031 32 102299032 33 102299033 34 102299034 35 102299035 36 102299036 37 102299037 38 102299038 39 102299039 40 102299040 41 102299041 Sarlaliat faxt MaOH Blank Typ HaOH Blank T0X14S-RBS10199-H20 Blk-12, SEE TOX14S-R3S10199-Saru Blk-12, SEE TOX14S-RTS10199-5aru Blk-12, SEC TOX145-RB510199-Sppb-12, SEE Standard TOX145-RB510199-10ppb-12, SEE Standard TOX145-RBS10199-25ppb-12, SEE Standard TQX14S-RBS1Q199-S0ppb-12, SEE Standard TOX145-RBS10199-100ppb-l2, SEE Standard TOX14S-RBS10199-250ppb-12, SEE Standard TOX14S-ABS10199-500ppb-12, SEE Standard TOX14S-RBSlQ199-750ppb-12, SEE Standard TOX145-RBS1019-1000ppb-12, SEC Standard MaOH Blank TOX145-RTS-9B03245M, Dayl, 5ag/kg, D5O-axtl0/l9/99 T0X145-RTS-9B0324CM, Dayl, &ag/kg, DSO-axt10/19/99 TOX145-RTS-9B03247M, Dayl, Smq/kq, D50-axt10/19/99 TCQU4S-RTS-9R03248M, Dayl, Sng/kg, DSO-axt10/19/99 TQX14S-RTS-9R03249M, Dayl, 5ag/kg, DSO-axtlO/19/99 rO X 1 4 5 -R B S 1 0 l9 9 -2 5 O p p b - C C V - ll-l, SEE oc MaOH Blank TOX14S-RTS-9R032SQM, Day4, 5ag/kg. DSO-axt10/19/99 TOX145-RTS-9R03251M, Day4, Sng/kg, DSO-axt10/19/99 TOXI45-RTS-9R032S2M, Day4, Sng/kg, D50-xt10/19/99 TOX145-RTS-9R032S4-IM, Day4, 5ag/kg, 050- 10/19/99 TOX14S-RTS-9R03254-2M, Day4, Sag/kg, 050- 10/19/99 TOX145-RBS1199-250ppb-CCV-l1-2, SEE OC MaOH Blank TOX145-RB510199-H2O Blk-12, SEC TOX14S-RBS:0199-Srua Blk-12, SEE TOX14S-RTSI0199-5aru Blk-12, SEE TOX14S-RBS10199-5ppb-12, SEC Standard TOX145-RBS10l99-1Oppb-12, SEE Standard TOX145-RB51Q199-25ppb-12, SEE Standard TOX145-RBS10199-50ppb-12, SEE Standard TOX145-RB510199-10Oppb-12, SEE Standard TOX14S-RB310199-2S0ppb-L2, SEE Standard TOX145-RBS10199-500ppb-12, SEE Standard TOX145-RBS10199-750ppb-12, SEE Standard TOXI45-RBS10199-1OOOppb-12, SEE Standard Std Cone 4.93 9.77 24.90 49.30 97.70 248.00 493.00 736.00 977.00 248.00 248.00 4.93 9.77 24.00 49.30 97.70 246.00 493.00 736.00 977.00 RT 7.946 7.840 7.943 7.850 7.043 7.926 7.834 7.840 7.828 7.821 7.920 7.026 7.926 7.035 7.053 7.925 7.826 7.925 7.825 7.042 7.924 7.868 7.849 7.033 7.S4B 7.845 7.850 7.628 7.852 7.946 7.853 7.843 7.826 7.027 7.051 7.828 7.630 7.846 7.828 7.827 7.832 Arta 465 331 152 151 95 915 1344 3615 5624 10036 39992 80296 126147 170989 424 1404 2212 1199 1612 1370 219 37 330 316 396 422 337 283 25 61 47 56 730 1319 3425 5469 18963 41057 69564 125699 168896 Cene. Plaga %Dav 4.23 bb 3.42 bd 2.33 MK 2.33 MM 1.99 MM 6.36 bb 29 9.57 bb -2 23.35 bb -6 35.54 bb -28 110.89 bb 13 244.14 bb -2 537.25 bdX 9 767.03 bbX 4 1039.19 bbX 6 3.98 bb 9.94 bb 14.63 bb 8.69 bb 11.19 bb 9.72 bb 2.73 bb -99 1.63 bb 3.42 KM 3.33 bb 3.92 bb 3.97 MM 3.46 bb 3.13 bb -99 1.56 bb 1.78 MM 1.70 M4 1.75 MM 5.84 bb 19 9.41 bb -4 22.20 bb -10 34.60 bb -30 116.50 bb 19 250.60 bb 1 538.93 bbX 9 764.31 bbX 4 1026.49 bbX 5 Paga 3 illa 062498: Quantitatad and Printad by iaa 10/25/99 /% Quantify Compound tiaamry tepore TOX145-rat aarua dilutiona, day 1 ( 4 - ext. 10/19/99 SEX Saaplo Lit: C :\>ftS.T\amna-rate.P*O\SanplOB\102299a Late attdi.fiad: Mon Oet 2S 09:43:56 1999 Method: C:\MMBLTICC\aattlia-rata.fRO\NethDB\102299a Laae mdlfted: Mon Oet 25 09:39:55 1999 Jota Codo: Printed: ten Oet 25 09:59:42 1999 Ccepound 4 : IS (Ch3) 4 Ham 1 102299001 2 102299002 3 102299003 4 102299004 5 102299005 6 102299006 7 102299007 0 102299008 9 102299009 10 102299010 11 102299011 12 102299012 13 102299013 14 102299014 15 102299015 16 102299014 17 102299017 18 102299018 19 102299019 20 102299020 21 102299021 22 102299022 23 102299023 24 102299024 25 102299025 26 102299026 27 102299027 28 102299028 29 102299029 30 102299030 31 102299031 32 102299032 33 102299033 34 102299034 35 102299035 36 102299036 37 102299037 38 102299038 39 102299039 40 102299040 41 102299041 Ba^leliat Teat Typ MeOH Blank MeOH Blank TOX145-RB510199-K2O BU-12, SEE TOX14S-RBS10199-Sens Blk-12, SEE TQX145-RTS10199-Seriai Blk-12, SEE TOX145-RBS10199-5ppb-12, SEE Standard TOX14S-RBSlQ199-10ppb-12, SEE Standard TOX145-BBS10199-25ppb-12, SEE Standard TOX145-RBS10199-50ppb-12, SEE Standard TOX14S-RBS10199-10Oppb-12, SEE Standard TOX145-RBS10199-250ppb-12, SEE Standard TOX145-RB$10199-500ppb-12, SEE Standard TOX145-BBS10199-7SOppb-12, SEE Standard TOX145-RBS10199-1000ppb-12, SEE Standard MeOH Blank TOX145-RTS-9R0324SM, Dayl, Seg/kg, DSO-axClO/19/99 roxi45-RTS'M03249M, Dayl, 5ag/kg, DSO-axtlO/19/99 TQX14S-RTS-9R03247M, Dayl, Seg/kg, DSO-axtlO/19/99 TOX145-RTS-9R0324SM, Dayl, 5*g/kg, D50-xtl0/19/99 TOX145-RTS-9R03249M, Dayl, 5*j/kg, DSO-axtlO/19/99 T0X14S-RBS1019B-2S0ppb-CCV-ll-l, SEE QC MaOH Blank TOX14S-RTS-9R032S0M, Day4, Seg/kg, D50-axtl0/19/99 TOX145-RTS-9R03231M Day4, Sag/kg, DSO-axtlO/19/99 TOX145-RTS-9R032S2M, Day4, Seg/kg, DSO-axtlO/19/99 T0X14S-RTS-9R03254-1M, Oay4, Sag/kg, D50- 10/19/99 T0X145-RTS-9R03254-2M, Day4, Sag/kg, D50- 10/19/99 TOX145-RB510199-250ppb-CCV-ll-2, SEE QC MaOH Blank TOX14S-RBS10199-H2O Blk-12, SEE T0X14S-RBS10l99-Srua Blk-12, SEE TOX145-RTS10199-Sarua Blk-12, SEE TOX14S-RBS10199-5ppb-12, SEE Standard TOX14S-RBS10199-10ppb-12, SEE TOX145-RBS10199-25ppb-12, SEE Standard Standard TOX145-RBS10199-50ppb-12, SEE Standard TOX145-R3S10199-100ppb-12, SEE Standard TOX14S-RBS10199-2SOppb-12, SEE Standard T0X14S-RB510199-500ppb-12, SEE Standard TOX145-RS10199-7S0ppb-12. SEE Standard TOX145-RBS10199-1000ppb-12, SEE Standard Btd Cone 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 RT 7.001 9.984 7.002 9.988 7.014 6.997 7.009 7.000 6.983 9.985 9.983 9.994 9.984 9.985 9.982 6.982 6.976 6.983 6.982 6.987 6.983 7.003 6.983 6.985 6.981 6.987 7.001 6.983 6.988 7.009 7.007 7.012 7.004 7.009 7.008 6.991 A r m Cone. Plaga tOv 3036 2591 2851 2705 2805 2491 2154 2852 2809 3031 3075 2977 89 93 76 76 69 2290 84 58 90 66 70 1999 2798 2329 2521 2515 2308 2391 2192 2855 2958 2896 2813 2853 1.13 bd 0.96 bb 1.06 bb 1.00 bb 1.04 bb 0.93 bb 0.80 bb 1.06 bb 1.04 bb 1.13 dd 1.14 bd 1.11 m 0.03 fi 0.03 MM 0.03 bd 0.03 bd 0.03 bb 0.95 bb 0.03 bb 0.02 bd 0.03 KM 0.02 bd 0.03 bd 0.70 bb 1.04 bd 0.96 bb 0.94 bb 0.93 bd 0.86 fi 0.89 bd 0.91 bd 1.06 bb 1.10 bd 1.08 bd 1.04 bd 1.06 bb 13 -4 6 0 4 -7 -20 6 4 13 14 11 -97 -97 -97 -97 -97 -15 -97 -98 -97 -98 -97 -30 4 -14 -6 -7 -14 -11 -19 6 10 8 4 6 Pag 4 A m i l a 092490: Quantitated and Printed tay laa 10/25/99 000605 __ ___________ _____________________________________________ ,__________________________________________________ '%-* Quantify Calibration Mp o r t TOX14S~rat aoraa dilution, day 1 4 4* oat. 10/19/ SIS Compound 1 name: POAA (C hi) Response Factor 115.846 Response type: External Std, Area Curve type: RF '-- y1 ~~ 000606 B E S T C O P Y A V A IL A B L E Quantify Calibration Report TOX14S>rat M r dilutiona, day 1 * < oat. 10/11/ SSI Compound 2 name: PFOS (Ch2) ' Coefficient of Determination: 0.995295 Calibration curve: 44.8833 * x + 108.462 Response type: External Std, Area Curve type: Linear, Origin: Exclude, W eighting: 1/x, Axis trans: None Pag 2 000607 BEST COPY a v m iu t w D M I W W I r* Quantify Calibration *aport T0X14S~rat aarua dllutiona, day 1 4 4* axt. 10/19/99 9BK Compound 3 name: PFOSA (Ch4) ' Coefficient of Determination: 0.989156 Calibration curve: 164.764 * x + -232.515 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None 9*9 3 BEST COPY available 000608 b e s t COPY AVAILABLE Quantify Calibration ftspore TOX145-rat i t n a dilutions, day I M - oat. 10/19/99 SXC Compound 4 name: IS (Ch3) Response Factor: 2692.44 Response type: External Std, Area Curve type: RF 3.07e3 **9* 4 X Response- 000609 Method Report Machod fila: Last modified: Compound: Printed: C :\HASSLTNX\ameUa-rats.PRO\MethD8U02299a.mdb Mon OcC 25 06:39:55 1999C 1: POAA (Chi) Kon OcC 25 07:03:23 1999 Compound Name: Internal Ref.: Quantify Traca: Cone, of scandarda: User RP Valua: User Peek Factor: Integrate Window Factor: Chromatogram mass window: Paak Location Retention Tima {mins): Relative Retention Time: RT Reference: Time Window (mins): Paak Selection: Response Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Concentration Units: Noise Peak-to-peak amplitude: Smooth Smoothing: Window site (scans): Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: Peak Separation Draw vertical threshold: Cetact shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative area: Absolute area: PQAA IChl) [None) TIC Fixed 1.000000, Disabled 1.000000 2.000 l.OOOODa 6.994, Enabled 0.000, Disabled [None] 0.203 Nearest External Areas Linear Exclude 1/X None 95 Disabled 2 1 30.00 200.00 5.00 90.00 Disabled 30.00 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled Aw/i DL&ii Page l 000610 Method Report Method file: Lest Modified: Compound: Printed: C:\KASSLYNX\amella-rate.PRO\MethDB\102299a.mdb Mon Oct 25 06:39:55 1999C 2: PFOS <Ch2> Mon Oct 25 03:03:23 1999 Coapound Name: Internal Ref.: Quantify Trace: Cone, of Standard: User RF Value: User Peat Factor: Integrate Window Factor: Chromatogram m s s window: Peak Location Retention Time (mins): Relative Retention Time: RT Reference: Tiae Window (sins): Peak Selection: Resoonae Response Type: Reaponee: Calibration Curves Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Concentration Units: Noise Peak-to-peak amplitude: Smooth Smoothing: Nindow size (scans): Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raisa baseline maximum: Peek Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative ares: Absolute area: PFOS <Ch2) (None] TIC Cone. A 1.000000, Disabl 1.000000 2.000 l.OQOODe 7.170, Enabled 0.000, Disabled [None] 0.262 External Areas Linear Exclude 1/X Nona 2300 Disabled 2 1 30.00 200.00 5.00 90.00 Disabled 30.00 1.50, Disabled o.oo. Disabled 2.00, Disabled 0.00, Disabled Fade 2 A * J * M f S w l '/ t f l f l 000611 Method Report Method file: Lest modified: Compound: Feinted: C:\HASSLWtt\aMna-rats.PRO\MethDB\102299a.mdb Mon Oct 25 06:39:55 1999C 3: PFOSA ICh4) Mon Oct 25 07:03:23 1999 Compound Name: Internal Ref.: Quantify Trace: Cone, of Standards: User RP Value: User Peak Factor: Integrate Window Factor: Chromatogram m s s window: Peak Location Retention Time (mins): Relative Retention Time: RT Reference: Time Window (minal: Peak Selection: Response Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Concentration Units: Noise Peak-to-peak amplitude: Smooth Smoothing: Window site (scans): Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raisa baaeline maximum: Peak Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative area: Absolute area: PFOSA (CM) (None] TIC Cone. B 1.000000 Disabled 1.000000 2.000 1.00000a 7.846, Enabled 0.000, Disabled (None) 0.273 External Areas Linear Exclude 1/X None 1(1 Enabled 2 1 30.00 200.00 5.00 90.00 Disabled 30.00 1.50, Disabled 0.00, Disabled 2.00. Disabled 0.00, Disabled /bu/i. Page 3 X* 000612 Mathod Report Method file: Last modified: Compound: Printed: C:\MA5SLYNX\amallatrate.PRO\MethO0\lO2299a.mdb Mon Oct 25 06:39:55 1999G 4: IS (Ch3) Mon Oct 25 07:03:23 1999 Compound Name: Internal Raf.: Quantify Trace: Cone, of Standards: User RF Value: User Peak Factor Incerate Window Factor: Chromatogram aas window: Peek Location Retention T m a Imins) : Relativ Retention Tim: RT Referance: Time Window (ins): Peak Selection: Rasponea Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Concentration Units: Noise Peek-tO'paak amplitude: Smooth Smoothing: Window aire tacana): Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peek tailing: Raise baseline maximum: Peak Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative area: Absolute arse: XS (Ch3) (Nona] TIC Fixed 1.000000, Disabled 1.000000 2.000 l.OOOODa 7.040, Enabled 0.000, Diaabled (None] 0.239 Nearest external Areas Linear Exelude 1/X None 99 Diaabled 2 1 30.00 200.00 5.00 90.00 Disabled 30.00 1.50, Disabled 0.00, Diaabled 2.00, Diaabled 0.00, Diaabled Page 4 a v f n -JSts ,a/ g e / f 7 000613 AMELIA 062498: FACT Equipment Log 99114 Q uattro n, #6448E PAGE DATE: 10/22/99 ANALYST: ias STUDY NUMBER: TOX145 MATRIX: Rat sera DESCRIPTION: Day 1&4 dilutions FACT Method: ETS-8-5.1 Injection volume: 10 uL Cycle time: 10 min. Electrode: Z-Spray Mobile Phase: (A)2.0 mM NH4CH3CQ2 TN-A- or stndrd number (A) 99085-10-14 (B) MeOH (B) TN-A-2945 Prepared (date/by): (A) 10/16/99 sah (B) 10/20/99 ias Expires: (A) 04/00______________ (B) 04/00 Store at room temp? 0 or N Other G uard column: None__________________ Part number: na_________ Lot number: na Analytical column: Keystone Bctasil ________________________ Size: 2 x 50 mm________________ Type: C18___________ Sphere size: 5 urn______ Part number: 055-701-2__________ Lot number: P9E11 Serial number:0591816Z Analytical parameters: Drying gas (L/hr): 300 ESI nebulizing gas (L/hr) 10 LC Flow rate: 300 uL/min. Back pressure: 62 bar Sheath gas (L/hr^0 HPLC solvent gradient: 10min-10-9S Time (min.) 1 ) 0.00___________ 2) 1.00_________ 3) 5.50_________ 4) 7.50_________ 5) 8.00_________ %B 10.0 10.0 95.0 95.0 10.0 1 4^ V u o BEST COPY AVAILABLE Tuning Method Report * Method: C :\MASSLYNX\AMELIA-RATS.PRO\ACQUDB\PFOSl-6KV Printed: Fri Oct 22 09:58:58 1999 Page 1 MS SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. Set Rdbk 1.60 40 5 0.2 150 250 1.60 -14 -4 149 253 Pressure* Analyser Vacuum Gas Cell Rdbk 1.2e-4 4.3e-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set Rdbk 15.0 15.0 2.0 0.0 4 650 7 Set Rdbk 14.0 14.0 10 2.0 0.0 40 0 650 41 38 40 000615 Scanning Method Report Method: C :\MRSSLYWC\AMRLIA-RhTS.PRO\ACQUDB\1OMZN-PTM-POAA> IS-PTO^A. Lest Modified: Mon Oct U 09:22:1? 1999 Printed: m Oct 22 09:S9:O9 1999 Solvent Delay ( eine > : 0.00 function : 1 M M of 1 Pteea Pair ( IIP- ) Inter Channel Delay [ Secs ) : 0.03 Span ( Daltons ) : 0.00 Start Ties ( Mins ) : 0.00 Cnd Tie* ( Mins ) : 10.00 Repeats : 1 Channel Patent Daughter Dwell (Secs) Coll Energy (eV) Cone ( V ) l 413.00 169.00 0.30 30 15 Function : 2 M M of 1 Mess Pair ( SSP- ) Inter Channel Delay ( Secs ) : Span I Daltons ) : Start Time ( Mins ) : End Tine < Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Sees) Coll Energy (eV) Cone 1 499.00 99.00 0.30 45 60 Function : 3 MRM of 1 Mass fair < **P- > Inter Channel Delay ( Secs ) : Span ( Daltons ) : Start Tie* ( Mins ) : End Tine ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) Coll Energy (eV) Cone 1 427.00 90.00 0.30 40 60 function : 4 MRM of 1 Mesa fair ( *99- ) Inter Channel Delay ( Seca ) : Span ( Daltons ) : Start Tine ( Hina ) : End Tine ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) Coll Energy (eV) Cone 1 496.00 79.00 0.40 45 60 taft l 000616 Method Report Method File: Last Modified: Printed: c:\aasslynx\amelia-rats.pro\acqudb\10inin-10-95 Friday, October 22, 1999 09:56:35 Friday, October 22, 1999 09:59:25 Page 1 HP1100 LC Pump Initial Conditions Solvents A B% C% D% 90.0 10.0 0.0 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(#C) 0.300 10.0 0 400 30.0 30.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 5 entries which are : Time 0.00 1.00 5. SO 7.50 8.00 A% 90.0 90.0 5.0 5.0 90.0 B% 10.0 10.0 95.0 95.0 10.0 C% 0.0 0.0 0.0 0.0 0.0 D% 0.0 0.0 0.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 Pressure 400 400 400 400 400 HP1100 LC Pump External Event Timetable The Timetable contains 3 entries which are : Time Initial 0.00 0.10 Column Switch Contact1 Off Off Off On Off Off Contact2 Off On Off Contact3 Off Off Off Contact4 Off On Off HP1100 Autosampler Initial Conditions Draw Speed Eject Speed {(il/min) Draw Position (mm) Stop Time (mins) Injection Volume()il) Vial Number 200.0 200 0.00 9.00 10.0 13 000617 Masslynx Sample List Sam ple List: C :\M A S S LY N X \am elia-rats.P R O \S am pleD B \102299a.S P L Printed: Fri Oct 22 09:58:46 1999 Page 1 P age Position: (1 ,1 ) File Name File T ext MS File 1 102299001 M eO H Blank 10 M IN -P F O S -P O A A -IS -P F O S A 2 102299002 M eO H Blank 10 M IN -P F O S -P O A A -IS -P F O S A 3 102299003 TO X145-RBS10199-H2O Blk-12, SEE 10M IN -P F O S -P O A A -IS -P F O S A 4 102299004 TO X145-RBS10199-Serum Blk-12. SEE 1 0 M IN -P F O S -P O A A -IS -P F O S A 5 102299005 TO X145-RTS10199-Serum Blk-12, SEE 1 0 M IN -P F O S -P O A A -1 S -P F O S A 6 102299006 TO X145-RBS10199-5ppb-12, SEE 1 0 M IN -P F O S -P O A A -IS -P F O S A 7 102299007 TOX145-RBS10199-10ppb-12, SEE 10M IN -P F O S -P O A A -IS -P F O S A 8 102299008 TOX145-RBS10199-25ppb-12, SEE 10 M IN -P F O S -P O A A -IS -P F O S A 9 102299009 TO X145-RBS10199-50ppb-12, SEE 10M IN -P F O S -P O A A -IS -P F O S A 10 102299010 TO X145-RBS10199-100ppb-12, SEE 10 M IN -P F O S -P O A A -IS -P F O S A 11 102299011 T O X 1 45-R B S 101 99-250 p p b -12 , S E E 10 M IN -P F O S -P O A A -IS -P F O S A 12 102299012 TO X145-RBS10199-500ppb-12, SEE 10 M IN -P F O S -P O A A -IS -P F O S A 13 102299013 TO X145-RBS10199-750ppb-12, SEE 10M IN-PFO S-PO AA-IS-PFO SA 14 102299014 TOX145-RBS10199-1000ppb-12, SEE 10 M IN -P F O S -P O A A -IS -P F O S A 15 102299015 M eO H Blank 10 M IN -P F O S -P O A A -IS -P F O S A 16 102299016 T O X 1 4 5 -R T S -9 R 0 3 2 4 5 M , D ay1, 5mg/kg, D 50-ext10/1 9/99 10M IN -P F O S -P O A A -IS -P F O S A 17 102299017 TO X145-R TS-9R 03246M , Day1, 5mg/kg, D50-ext10/19/99 10M IN -PFO S-PO A A -IS-PFO SA 18 102299018 T O X 1 4 5 -R T S -9 R 0 3 2 4 7 M , D ay1, 5mg/kg, D 50-ext10/1 9/99 10 M IN -P F O S -P O A A -IS -P F O S A 19 102299019 T O X 1 4 5 -R T S -9 R 0 3 2 4 8 M , D ay1, 5m g/kg, D 50-ext10/19/99 10M IN -P F O S -P O A A -IS -P F O S A 20 102299020 TO X145-R TS-9R 03249M , D ay1,5m g/kg, D50-ext10/19/99 10M IN-PFO S-PO AA-IS-PFO SA 21 102299021 TO X 1 45-R B S 101 99-250 p p b -C C V -11-1, S E E 10M IN -P F O S -P O A A -IS -P F O S A 22 102299022 M eO H Blank 10M IN -P F O S -P O A A -IS -P F O S A 23 102299023 T O X 1 4 5 -R T S -9 R 0 3 2 5 0 M , D a y4 ,5m g /k g , D 50-ext10/19/99 10M IN -P F O S -P O A A -IS -P F O S A 24 102299024 TO X145-R TS-9R 03251M , Day4,5m g/kg, D50-ext10/19/99 10M IN-PFO S-PO AA-IS-PFO SA 25 102299025 TO X145-R TS-9R 03252M , Day4,5m g/kg, D50-ext10/19/99 10M IN-PFO S-PO AA-IS-PFO SA 26 102299026 TO X145-R TS-9R 03254-1M , Day4, 5mg/kg, D 5 0 -10/19/99 10M IN-PFO S-PO AA-IS-PFO SA 27 102299027 T O X 1 45-R T S -9R 032 54-2M , D ay4, 5mg/kg, D 5 0 - 10/19/99 10M IN -P F O S -P O A A -IS -P F O S A 28 102299028 TO X 145-RBS10199-250ppb-CCV-11-2, SEE 29 102299029 MeOH Blank 10M IN -P F O S -P O A A -IS -P F O S A 1 0 M IN -P F O S -P O A A -IS -P F O S A 30 102299030 TO X145-R B S10199-H 2O Blk-12, SEE 1 0 M IN -P F O S -P O A A -IS -P F O S A 31 102299031 T O X 1 45-R B S 101 99-S e ru m B lk-12. S E E 32 102299032 TO X145-RTS10199-Serum Blk-12, SEE 33 102299033 TOX145-RBS10199-5ppb-12, SEE 34 102299034 TO X145-RBS10199-10ppb-12, SEE 35 102299035 TO X145-RBS10199-25ppb-12, SEE 36 102299036 TOX145-RBS10199-50ppb-12, SEE 37 102299037 TO X145-R B S10199-100ppb-12, SEE 38 102299038 TO X145-RBS10199-250ppb-12, SEE 39 102299039 TO X145-RBS10199-500ppb-12, SEE 40 102299040 TO X145-RBS10199-750ppb-12, SEE 41 102299041 TO X 145-R B S 101 99-100 0p p b -1 2, S E E 1 0 M IN -P F O S -P O A A -IS -P F O S A 1 0 M IN -P F O S -P O A A -IS -P F O S A 10 M IN -P F O S -P O A A -IS -P F O S A 1 0 M IN -P F O S -P O A A -IS -P F O S A 10 M IN -P F O S -P O A A -IS -P F O S A 10M IN -P F O S -P O A A -IS -P F O S A 1 0 M IN -P F O S -P O A A -IS -P F O S A 10 M IN -P F O S -P O A A -IS -P F O S A 10 M IN -P F O S -P O A A -IS -P F O S A 1O M IN-PFO S-PO A A -IS^PFO SA 1 0 M IN -P F O S -P O A A -IS -P F O S A 000618 Masslynx - Sample U at Sam ple List: C :\M A S S LY N X \am elia-rats.P R O \S am pleD B \102299a.SP L Printed: Fri Oct 22 09:58:46 1999 Page 2 P age P osition-12 1) '' ' Inlet File Bottle Inject Volum e Sam ple Type Cone A Cone B Cone C C one D C on e E Cone F 1 10m in-10-95 91 2 10m in-10-95 91 3 10min-10-95 1 4 10min-10-95 2 5 10min-10-95 3 6 10min-10-95 4 7 10min-10-95 5 8 10mirv-10-95 6 9 10min-10-95 7 10 10min-10-95 8 11 10m in-10-95 9 12 10mitv10-95 10 13 10min-10-95 11 14 10min-10-95 12 15 10min-10-95 92 16 10miri-10-95 13 17 10min-10-95 14 18 10min-10-95 15 19 10min-10-95 16 20 10min-10-95 17 21 10m in-10-95 33 22 10mir>10-95 92 23 10rron-10-95 18 24 10min-10-95 19 25 10min-10-95 20 26 10min-10-95 21 27 10min-10-95 22 28 10min-10-95 34 29 10min-10-95 93 30 10mirv-10-95 1 31 10min-10-95 2 32 10min-10-95 3 33 10min-10-95 4 34 10min-10-95 5 35 10mir>-10-95 6 36 10min-10-95 7 37 10min-10-95 8 38 10mirv-10-95 9 39 10min-10-95 10 40 10mirv10-95 11 41 10min-10-95 12 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 000619 FACT: DATA REVIEW SUMMARY FORM Date: Data Analyst: FACT Study H: Matrix/Timepoints: Sample List /ZZ22&_______ / < 3lS ? 9b _________________________ Set-up Analysis Date/Analyst: Instrument , 0 ? / / ? / t e / < 9 9 _____ --Analyte: Tjgas ***> Data Review Sign-Off i Analyst Review Name/ Date: / ' '7 / f \ v s s r s m -^ Quality Assurance Review Name / Date:____________ i kh Data E ntry:. (AL ll& hi Comments / Justifications: n Y Q /tGjL____ / - y L O Q :_ R"2: 4 ^Extraction Blank: Matrix Blank: ' k f J X X Calibration Checks: MSMsn______ H lA - .- m nr Data Status:: < ) n a ly u J i* H* U JViyLhi l A l idwlfi ( /k > / * * p / 2' ~ # p h / i J - / d f x x a C , , S ^ ^ JTueAfY Aa*JZ' P / s s / / / y J ^ / /& ,& p M ? ~ ^ tfXLt?=i.________________________________ ^ Analyte: Acceptable Linear Range: ^7* /) LOQ: p/ Wo ho Extracted Blank: ^ Matrix Blank: // k Calibration Checks: / 7 A ^ _________________________________ M S /M S D :______________ D a k Data Status: H fi U d I U ie A a im . n ^ W - _____l a l f l f o /Th^^/f/AJhr7AO (f&i/ /2srtSlA /. 'df-hp u n f- Ljn h? &nP* / / / %)t JS ..C?,, Analyte: Calibration Checks: M S /M S D :________ Data Satus: Extracted Blank: _ Matrix Blank: < 0y Z 000620 i i * 9 I i 00062X l,..- 'V, ,>: K ft f IAIA n ff 55555 55555 SS33 33333 8888 88 I 535352.. SSSgSSS 5355 gggg 55 535352.. gg ggggssssa SSSSSSSSSSSSSSSSSgSSSSSSSgSS i i S S ^ c S i i i i i i i S3 i i 3 - i 3 i S S E S Ss SSSHSsss.--- sssSsSSSS-HSSSSSSJSssass.......... 8 S335K53g53 53SgSS5SSS3 3S33SS3g3gt5g233bbt!SSJ? 583CSBg KCm S i . ...3SS f VJ _> ! o I 9 I 8 oO o O fO 33333 53-33 i 8888 88 ? p iiiii liiili o 1. *7TM" SSsSSS.. SSSS SS SSS3SS-. SSSS3S535 SSSS SS SSSSSSSSS -J> 1 . ggiiSSsiSE3EgggEE3EEl a . 3B338S33g3SS&333385eSe33BBB33SB8B8SBBBBge3&S3 P SSSHSsgB.-.wSsrs.......... Ss.s.e.JsssSSKSs...........y I g^pssfcsssisssEKsassssssssssBgpsissbbssassssbf ,,,,.,,,,SSiS S i- KSi-S i oo o 05 O co OOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOO' ;s e | MMMMUMMMMMMWWMWMNMMWMMMMMMNMMMMMMMMMMMMI jmmi U ' UMA U> t X Ut V> U> I XWl UI U* UI U* Ul t A UI UI UI UI UI UMa u l UI MUI UI UI UI UI UI UMl U I U I I * U I U l U t U M * Uv m. l_ ooooooooooooooooooooooooooooooooooooooooooooo WMPOVA'JAWAWMHOiaA-JAV^UMHOKA'JAW^b'MHOVn'IOUO^UWMO o 3 3 3 3 3 3 3 3 3 3 3 3 8 3 3 3 3 3 3 3 3 3 1 3 8 3 3 3 3 3 1 3_ 8 3 3 8 3 3 B s s B B B E B B B B B g B B E E B B B B B i B S B B B B B S EBBBBBBBC lili p r p z> p,, O r* \ Op gggggggggggg&gggg333mgg33333gggggggggggggm ooooeoeoooeo oooo* USEUS5S555U5 EAS'SAISAS'ASWSWWSWSW B MNMMUIiy!IW es uo<s*ws ws sws I wM wM wM wU wM M h*> `S8BSC oooooooooooc f i f i SSi i7 7 Siitt . L C C w *M h h T Q Q H `Q O D `<S*< H *** CCBf 77C S BB B8 b s b b ? -%S HC Gas?r r jfmjfir **"w BB -:|m &b?i i i i i ?m ? gssassss5G.G MMB BB BB ss sisr SS555 sssss 8888 :s 33333 88 3 cr sr S- c- -e> To googooggg gggg ss g3BgSgSSSSSSSSSSSSSSSSSSSSSSSSS Hs ^ s s i i2 ! O J i s J i . J i s y i i 3 i i A S g g g & 5 5 m S S m S 5 5 5 5 g S S m & 8 5 & & m S & & g & 5 m 53 ilBgSSS53SBSg5gSSSS5SSSSS3BSBSSSSS3B33BSSSB B i i 33S33 i w tr ! Ouaaclfy Calibration U p o n n x 145: ma sraP say 144 dilations, feet 10/19/99 CC0S24 Quantify calibration Roport ten 145: bat tara. Day 1 M dilatioaa, Rxt 10/19/55 a 000625 Quantify Calibration u p o n on 14S: Rat Sara, Day 1*4 dilutions, Uct 10/19/ Saos 3 rr? 6 2 G Method Report Method fil: Last modified: Compound : Printed: C:\MRSSLYia\soup020199.pro\MethDBU02599b.mdb TU Oet 2< 09:11:31 1999 1: FFOS Tua Oet 2 10:40:14 1999 Compound I M : Internal Ref.: Quantify Trac: Cene, of Standard: Osar RP Valu: User Peak Factor: Integrate Window Factor: Chromatogram mass window. pros [Io m ] TIC Coac- A 1.000000, Diaablad 1.000000 2 .0 0 0 l.OOQOOa Retention Time (mine} : Relative Retention Time: RT Reference; Tiaw Window (mina) : Peak Slction: 7.490, Bnabled 0.000, Diaablad (Won] 0.312 Waaxat Response Typa : R*apona: External Aroaa Polynomial iypa: Point of Origin: Fit Weighting: Axia Transformation: linear include 1/X Io m Units: Peak-to-peak anplituda: 76 Smoothing: Window aix (acana): Number of mnrtrht Smoothing method: babied 2 1 Join vally threshold: Raduca peak tailing: Rais baseline maxim: 30.00 200.00 5.00 Draw vertical threshold: Detect shoulders: Shoulder threshold: 90.00 Disabled 30.00 Relative height: Absolute height: Relative area: Absolute area: 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled j J 2 //3 Pag 1 000627 Nathod Report Method file: Last modified: Ccwpouad: Prinead: C:\KASSLYMX\eoup020199.pro\MethDa\102S99b.ndb Tua Oct 26 09:11:21 1999 2: PPOSA Tua Oct 26 10:41:14 1999 Compound Mama: Internal Raf.: Quantify Traca: Cone, of Standards: Usar Mr Valua: User Peak factor: Integrate window factor: Chromatogram mass window: PPOSA [None] TIC Cone. S 1.000000. Disabled 1.000000 2.000 l.OOOODa Retention Tina (mine}: Relative Retention Tina: RT Rafaranca: Tina Window (mins): Peak Selection: 7.940, Enabled 0.000. Disabled (None) 0.400 Nearest Response lypa: Response: Bxtemal Areas Polynomial Type: Point of Origin: Pit Weighting: Axis Transformation: Linear Exclude 1/X None Units: Peak-to-peak aag>litude: 74 Smoothing: Window sisa (scans): Number of smooths: Smoothing method: Enabled 2 1 Join valley threshold: Reduce peak tailing: Raise baseline maximum: 20.00 200.00 5.00 Draw vertical threshold: Detect shoulders: Shoulder threshold: 90.00 Disabled 20.00 Relative height: Absolute height: Relative area: Absolute ares: 1.S0, Disabled 0.00. Disabled 2.00, Disabled 0.00. Disabled > MO 2 000628 Nathod Raport Kathod Cila: Laat difiad: Compound: Printed: C:\MAS5LYlGC\aoup020199.pro\MathDS\102599b.adb Tua Oct 2$ 09;U:31 1999 3; Surr Tua Oct 2< 10:49:14 1999 Coopound Name: Internal Pat.: Quantify Trace: Cone, of Standarda: Uaar HP Valua: Uaar Peak factor: Integrate Window Factor: Chromatogram maaa window: Surr IMona] TIC Fixed 1.000000, Oiaablad 1.000000 2.000 l.OOOODa Katantion Tina (nina): Ralativa Ratantioa Tina: RT Rafaranca: Tina Window (nina): Peak Salaction: 7.245. Snablad 0.000. Oiaablad (Hone) 0.301 Nearest Raaponaa Typa: Raaponsa: Kxtarnal Araaa Polynomial Typa: Point of Origin: Pit Waigbting: Axia Tranaformation: Llnaar Sxcluda 1/x Nona Onita: Faak-to-peak amplitude: Sacothing: Window aise (acans): Number of amootha: Smoothing method: 5 Snablad 2 1 Join vallay threshold: Raduca paak tailing: Raiaa baaalina a x i n a : 30.00 200.00 5.00 Draw vartical thraahold: Datact ahouldara: Shouldar thraahold: 90.00 Oiaablad 30.00 Ralativa haight*. Absolute haight: Ralativa araa: Abaoluta araa: 1.SO. Oiaablad 0.00, Oiaablad 2.00. Oiaablad 0.00, Oiaablad Paga 3 000629 /O Quattro II, #6414E SOUP 020199: FACT Equipment Log 99092 PAGE 1/1 DATE: 10-25-99 ANALYST :mmmh STUDY NUMBER: TOX145 MATRIX: Rat sera DESCRIPTION: Dilutions FACT Method: ETS-8-5.1 Injection volume: 10 uL Cycle time: 10 min. Electrode: Z-Sprav Mobile Phase: (A12.0 tnM NH4CH3C02 (B )MeOH TN-A-or stndrd number (A) 99085-11-3________ Prepared (date/by): (A) 10/21/99 mmh_______ (B)TN-A:28S?.. (B) 10/16/99 sah Expires: (A) 04/00______________ (B)_MQ______ Store at room temp? @ or N Other: G uard column: None__________________ Part number: na_________ Lot number: na Analytical column: Keystone Betasil___________________________________ Size: 2 x 50 mm________________ Type: CIS___________ Sphere size: 5 um Part number: 055-701-2__________ Lot number: P9E11 Serial number:0591804Z Analytical parameters: Drying gas (L/hr): 350 ESI nebulizing gas (L/hr) 13 LC Flow rate: 300 uL/tnin. Back pressure: 65 bar Sheath gas (L/hr)_Q____ HPLC solvent gradient: 10min-10-95 Tim? (min)___ DJLQQ________ 2) _LQQ_ 3 ) ^ 5 2 __________ 4 ) T5Q__ 5 1 M Q ____________ %B M Sl JOCL jia 25JL 1M_ 000630 BEST COPY AVAILABLE Tuning Method Report Method: C :\MASSLYMX\SOUP-RATS.PRO\ACQUDB\PFOS3 Printed: Mon Oct 25 16:37:32 1999 Page 1 MS SOURCE ( ESP- ) CapillaryCone Extractor RF Lens Source Block Temp. Desolvation Temp. MS Set Rdbk 1.60 60 5 0.2 150 250 1.60 -60 -6 151 250 Pressures Analyser Vacuum Gas Cell Rdbk 5.9e-5 4 .le-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set Rdbk 14.0 14.0 0.9 0.0 4 650 3 Set Rdbk 14.0 14.0 60 2.0 0.0 40 0 650 42 38 44 000631 leualao mthcd Mport i Mattedt cuaMLYxx\*oc-iu>TS.nt0\ACQOOM\ioiaM~rroa-Kut-rrocA-xa teat Modified: Pri Oet IS 11:39:03 1999 Printed: Maa oet 29 l:2t:24 1999 Solvent Dalny ( talan > ! 0.00 function : 1 M M of 1 Mk u pair ( - ) Intar Chennai Dalny ( Saca ) : Span { Dalton* ) : Start Tine ( Mina ) : End Tine ( Kina ) : Repeats : Channel Parant Daughter 0.03 0.00 Q.QQ 10.00 1 Dwell (Saca) Coll Energy (aV) Cone 1 413.00 169.00 0.30 30 15 function : 2 M M of 1 Mass pair ( MSP- ) Inter Channel Delay ( Secs ) : Span ( Dalton* } : Start Tiaa ( Mina ) ; End Tiaa ( Kin* } : Repeat* : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Seca) Coll Knergy (SV) Co bs 1( V 1 499.00 99.00 0.30 45 0 funetloa : 3 M M of 1 Maas pair ( BSP- ) Inter Channel Delay i( Secs > : Spaa ( Deltona ) : Start Tine ( Mina ) i Snd Tine ( Mina ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) Coll Bnergy <OV) Cone i( V 1 498.00 71.00 0.30 45 60 Function : 4 M M of 1 Mass pair { - ) Inter Channel Delay i[ Secs ) : Span ( Daltons ) : Start Tine { Mins ) : Bnd Tina < Kina ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) Coll Energy <eV) Cone 1( V 1 427.00 SO. 00 0-30 40 60 Method Report Method rilas Last Modified: Printed: c:\masslynx\soup-rata.pro\aequdb\iamin-10-95 Monday, October 25, 1999 16s29>5t Monday, October 25 1999 lSi34>4S HP1100 LC Puagp Initial Condition Solvents A% B% C% D% 90.0 10.0 0.0 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 0.300 10.0 0 400 30.0 30.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 5 entries which are : Time A% B% C% D4 0.00 90.0 10.0 0.0 0.0 1.00 90.0 10.0 0.0 0.0 5.50 5.0 95.0 0.0 0.0 7.50 5.0 95.0 0.0 0.0 8.00 90.0 10.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 h p i i o o l c pump Extar&Al Kvmsxt The Timetable contains 3 entries which are : Time Initial 0.00 0.10 Column Switch Contact1 Off Off Off On Off Off Contact2 Off On Off Contact3 Off Off Off Contact4 Off On Off HP1100 Autoaaapler Initial Conditions Draw Speed Eject Speed (pl/min) Draw Position (mm) Stop Time (mins) Injection Volume(iil) Vial Number 200.0 200 0.00 9.00 10.0 9 Pape 1 ^ & 5 = $ Pressure 400 400 400 400 400 000633 Masslynx - Sample List Sam ple List: C:\M ASSLYNX\soup-rats.pro\Sam pleDB\102599b.SPL Printed: Mon Oct 2 5 16:32:57 1999 Page 1 Page Position: (1 ,1 ) File Name File Text M S File 1 102599039 MeOH Blank 10M IN -P F O S -P O A A -P F O S A -IS 2 102599040 M eO H Blank 10M IN-PFOS-POAA-PFOSA-IS 3 102599041 TO X145-R B S1019 9 -H 2 0 Blk-12, SEE 10M IN-PFOS-POAA-PFOSA-IS 4 102599042 TO X145-R B S 10199-Serum Blk-12, SEE 10M IN-PFOS-POAA-PFOSA-IS 5 102599043 TO X145-R TS10199-Serum Blk-12, SEE 10M IN-PFOS-POAA-PFOSA-IS 6 102599044 TOX145-R8S10199-5ppb-12, SEE 10 M IN -P F O S -P O A A -P F O S A -IS 7 102599045 TOX145-RBS10199-10ppb-12, SEE 10M IN-PFOS-POAA-PFOSA-IS 8 102599046 TOX145-RBS10199-25ppb-12, SEE 10M IN-PFOS-POAA-PFOSA-IS 9 102599047 TO X145-R B S10199-S0ppb-12, SEE 10M IN -P F O S -P O A A -P F O S A -IS 10 102599048 TO X145-R B S 10199-100ppb -12, S E E 10M IN-PFOS-POAA-PFOSA-IS 11 102599049 T O X 14 5 -R B S 10199-250ppb-12, S E E 10M IN-PFOS-POAA-PFOSA-IS 12 102599050 T O X I 45-RBS10199-500ppb-12, SEE 10M IN-PFO S-PO AA-PFO SA-IS 13 102599051 TO X145-RBS10199-750ppb-12, SEE 10M IN-PFOS-POAA-PFOSA-IS 14 102599052 TO X145-RBS10199-1000ppb-12, SEE 10M IN-PFOS-POAA-PFOSA-IS 15 102599053 M eO H Blank 10M IN-PFOS-POAA-PFOSA-IS 16 102599054 T O X 145-R T S -9R 0 324 5M , Day1, 5mg/kg, D 50-ext10/1 9/99 10M IN -P FO S -P O A A -P FO S A -IS 17 102599055 TO X145-R TS-9R 03246M , Day1, 5mg/kg, D50-ext10/19/99 10M IN-PFO S-PO AA-PFO SA-IS 18 102599056 T O X 1 45-R T S -9R 032 47M , D ay1, 5m g/kg, D 50-ext10/1 9/99 10M IN -P F O S -P O A A -P F O S A -IS 19 102599057 TO X145-R TS-9R 03248M , D a y l, 5mg/kg, D50-ext10/19/99 10M IN -PFO S-PO AA-PFO SA-IS 20 102599058 TO X145-RTS-9R03249M , Day1,5m g/kg, D50-ext10/19/99 10M IN-PFOS-POAA-PFOSA-IS 21 102599059 T O X 1 45-R B S 10199-250pp b-C C V -11-1, S E E 10M IN-PFOS-POAA-PFOSA-IS 22 102599060 TO X145-RBS10199-250ppb-12, SEE 10M IN-PFOS-POAA-PFOSA-IS 23 102599061 M eO H Blank 10M IN-PFOS-POAA-PFOSA-IS 24 102599062 TO X145-RTS-9R03250M , Day4,5m g/kg, D50-ext10/19/99 10M IN-PFOS-POAA-PFOSA-IS 25 102599063 TO X145-R TS-9R 03251M , Day4, 5mg/kg, D50-ext10/19/99 10M IN-PFO S-PO AA-PFO SA-IS 26 102599064 T O X 14 5 -R T S -9 R 0 3 2 5 2 M , Day4, 5m g/kg, D 50-ext10/19/99 10M IN -P FO S -P O A A -P FO S A -IS 27 102599065 TO X145-R TS-9R 03254-1M , Day4, 5mg/kg, D 5 0 -10/19/99 10M IN-PFO S-PO AA-PFO SA-IS 28 102599066 TO X145-R TS-9R 03254-2M , Day4, 5mg/kg, D 5 0 -10/19/99 10M IN-PFO S-PO AA-PFO SA-IS 29 102599067 T O X 1 45-R B S 10 1 99 -250pp b-C C V -11-2, SEE 10M IN-PFO S-PO AA-PFO SA-IS 30 102599068 TO X145-RBS10199-250ppb-12, SEE 10M IN-PFO S-PO AA-PFO SA-IS 31 102599069 T O X 1 45-R B S 10 1 99-250pp b-C C V -11-3, S E E 10M IN -P F O S -P O A A -P F O S A -IS 32 102599070 TO X145-R B S10199-250ppb-CCV-11-4, SEE 10M IN-PFO S-PO AA-PFO SA-IS 33 102599071 M eO H Blank 10M IN -P F O S -P O A A -P F O S A -IS 34 102599072 TO X145-R B S1019 9 -H 2 0 Blk-12, SEE 10M IN-PFOS-POAA-PFOSA-IS 35 102599073 TO X145-R B S10199-Serum Blk-12, SEE 10M IN-PFO S-PO AA-PFO SA-IS 36 102599074 TO X145-R TS10199-Serum Blk-12, SEE 10M IN-PFOS-POAA-PFOSA-IS 37 102599075 TOX145-RBS10199-5ppb-12, SEE 10M IN-PFOS-POAA-PFOSA-IS 38 102599076 TOX145-RBS10199-10ppb-12, SEE 10M IN-PFOS-POAA-PFOSA-IS 39 102599077 TO X145-RBS10199-25ppb-12, SEE 10M IN-PFOS-POAA-PFOSA-IS 40 102599078 TOX145-RBS10199-50ppb-12, SEE 10M IN-PFOS-POAA-PFOSA-IS 41 102599079 TO X145-R B S 10199-100ppb -12, S EE 10M IN -P F O S -P O A A -P F O S A -IS 42 102599080 TO X145-RBS10199-250ppb-12, SEE 10M IN-PFOS-POAA-PFOSA-IS 43 102599081 TO X145-RBS10199-500ppb-12, SEE 10M IN-PFOS-POAA-PFOSA-IS 44 102599082 T O X 145-R B S 10199-750ppb-12, SEE 10M IN-PFOS-POAA-PFOSA-IS 45 102599083 TOX145-RBS10199-1000ppb-12, SEE 10M IN-PFOS-POAA-PFOSA-IS 000634 Masslynx - Sam ple List Sam ple List: C :\M AS S LY N X \soup-rats.pro\Sam pleD B \102599b.S P L Printed: Mon Oct 25 16:32:57 1999 Inlat Fils Bottle Inject Volume Sample Type Cone A ConeB Cone C 1 10m in-10-95 91 2 10m in-10-95 91 3 10m in-10-95 21 4 10min-10-95 22 5 10min-10-95 23 6 10min-10-95 24 7 10min-10-95 25 8 10min-10-95 26 9 10min-10-95 27 10 10min-10-95 28 11 10m in-10-95 29 12 10min-10-95 30 13 10m in-10-95 31 14 10nnin-10-95 32 15 10min-10-95 92 16 10min-10-95 33 17 10min-10-95 34 18 10m in-10-95 35 19 10min-10-95 36 20 10min-10-95 37 21 10m in-10-95 43 22 10min-10-95 29 23 10min-10-95 92 24 10min-10-95 38 25 10min-10-95 39 26 10min-10-95 40 27 10m in-10-95 41 28 10min-10-95 42 29 10m in-10-95 44 30 10min-10-95 29 31 10m in-10-95 45 32 10min-10-95 46 33 10min-10-95 93 34 10m in-10-95 21 35 10min-10-95 22 36 10min-10-95 23 37 10min-10-95 24 38 10min-10-95 25 39 10min-10-95 26 40 10min-10-95 27 41 10m in-10-95 28 42 10min-10-95 29 43 10min-10-95 30 44 10m in-10-95 31 45 10min-10-95 32 10 10 10 10 10 _ -- -- -- -- 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 10 10 -- _ 10 10 10 -- _ 10 QC 10 10 10 10 Q_C -- _ 10 10 10 _ -- 10 QC 10 Q C 10 Q C 10 10 10 10 10 _Q C _ _ _ 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard ___ ... _ _ ... ----_ ------ _ ---- 4.93 9.76 24.8 49.3 97.6 248 493 735 9_7 6 4.93 9.77 24.8 49.3 97.7 246 493 736 9_7 7 -- -- -- -- -- -- -- -- -- -- __ _-- _-- _-- _ ---- 248 2--4 8 248 2_4 8 -- _ _ ---- ___ --_ ... --_ ... _ ... ... 248 248 248 248 246 248 ... ... _ 24 8 2_4 8 _ ___ ... _ _ ... --_ _ 4.93 9.76 4.93 9.77 _ _ 24.8 49.3 24.8 49.3 ---- 97.6 97.7 246 248 493 493 735 976 736 977 -- Page 2 P age Position: (2 ,1 ) 0006: FACT: DATA REVIEW SUMMARY FORM Date: Data Analyst: FACT Study #: SL 'iY/</S' Malnx/Timepoints: tS {yo y'/yi.^ r'j day / ^ < / Sample List ? <9*7.A _______________ Set-up Analysis Date/Analyst: Instrument: Data ReviewSign-Off ' s s r X j * > '^ 9 N airn/D ate: l e L a k f j fc'A f f r g / f f Q uality A ssurance Review Name / D ate:_____________ Data Entry:. e J w ic i o M < h Comments/ Justifications: (b l/fflA/afaot <nt//ys*z*' ^ @ 4 p Q td S >M 'A & .2 ft o & r p ? ^ /ntL AoAyn ^ j/U S ahfvS- Jxw ualA U fa / &x - 0 4/ /QplSS;/n ^ ,J lh /lfa //V/rf Uto fanOZfiAxL/7/r> 0/ rk/w - S.a.,, Qu/Le. /p& k&A ^ /2//ui*kj--y^ \ # f ty j ,/) Wu S k . J jn*t% f /r r r \ ljl fsflonsf- Passed i W t w W ^ W / A j . A l o ^ r ptesr+rr //yj X M - C B oc- S / g Q - f O n r ^ Z c m A tJ/HZ 5 i G A t / i C * * T 000636 Quantify Ccayoraid Sumary Baport Tor 145: Sat Sara and Livar, Day 1 4 4 Saapla List: C:\MASSLYKX\Davy070799.P*O\SaaplaDSU02799b Last aodifiad: Thu Oet 28 09:14:03 1999 Mathod: C :\MASSLTXX\Davay070799. PBO\Mah0SU02799b Last aodifiad: Thu Oct 28 08:57:32 1999 Job Coda: Printad: Thu Oet 28 09:27:15 1999 -- zrP t Ceapound 1: P O M (fuiks 1) * Maaa 1 102799013 2 102799014 3 102799015 4 102799016 5 102799017 6 102799018 7 102799019 0 102799020 9 102799021 10 102799022 11 102799023 12 102799024 13 102799025 14 102799026 15 102799027 16 102799028 17 102799029 10 102799030 19 102799031 20 102799032 21 102799033 22 102799034 23 102799035 24 102799036 25 102799037 26 102799030 27 102799039 28 102799040 29 102799041 30 102799042 31 102799043 32 102799044 33 102799045 34 102799046 35 102799047 36 102799048 37 102799049 38 102799050 39 102799051 40 102799052 41 102799053 42 102799054 43 102799055 44 102799056 45 102799057 46 102799058 47 102799059 40 102799060 49 102799061 50 102799062 51 102799063 52 102799064 53 102799065 54 102799066 55 102799067 56 102799068 57 102799069 56 102799070 59 102799071 Saaplalist Tart MaOH Blank MaOH Blank TOXI45-RBS10229-H2O Blk-1, RWW TOXH5-BS10229-S*rua Blk-1, BMW TOX145-RBS10229-lppb-l, BMW T0X1I5-RBS10229-5ppb-l, RWW TOX1I5-RB510229-10ppb-l, BMW TOX145-BBS10229-2Sppb-l, RWW TOX145-RBS10229-50ppb-l, BMW TOX145-RBS10229-100ppb-l, BMW TOX145-BBS10229-25Oppb-l, RWW TOX145-RBS10229-500ppb-l, BMW TOX145-RBS10229-750ppb-l, RWW TOX14S-RBS10229-1000ppb-l, BMW MaOH Blank TOX145-RTS-9R03230H, Dayl, control,-axtlO/19/99 TOX145-RTS-9R03231M. Dayl, control,-a*tl0/19/99 TOX145-RTS-9R03232H, Dayl, control,-aatlO/19/99 TOX145-RTS-9R03233M, Dayl, control,-axtlO/19/99 TOX145-RTS-9R03234M, Dayl, control,-axtlO/19/99 TOXll5-RBS10229-250ppb-i, BMW MaOH Blank TOX145-RTS-9R03235M, Dayl, control,-axtlO/19/99 TOX145-RTS-9R3236M, Dayl, control,-sxtlO/19/99 TOX14&-RTS-9R03237M, Dayl, control,-axtlO/19/99 TOX14S-RTS-9R03238H, Dayl, control,-sxtlO/19/99 TOX145-RTS-9R03239M, Dayl, control,-sxtlO/19/99 TOX145-RB510229-250ppb-l, BMW MaOH Blank TOX145-RTS-9R0324SK, Dayl, Sag/kg, axtlO/19/99 T0X1I5-RTS-9R03246H, Dayl, 5g/kg, axtlO/19/99 TOX145-RTS-9R03247M, Dayl, 5ag/kg, axtlO/19/99 TOX1I5-RTS-9R03248M, Dayl, 5ag/kg, axtlO/19/99 TOXI15-RTS-9R03249M, Dayl, 5ag/kg, axtlO/19/99 TOX145-RBS10229-2S0ppb-l, BMW MaOH Blank TOX145-RTS-9R03250M, Dayl, 5*g/kg, axtlO/19/99 TOX145-RTS-9R03251M, Dayl, 5ag/kg, axtlO/19/99 TOX14S-RTS-9R03252M, Dayl, 5ag/kg, axtlO/19/99 TOX145-RTS-9R03254-LM, Dayl, 5atg/kg, axt 10/19/99 TOX145-RTS-9R03254-2M, Dayl, 5ag/kg, axt 10/19/99 TOX145-R8510229-250ppb-l, BMW MaOH Blank TOX145-RTL-9R03247-M, Dayl, 5ag/kg, axt 10/13/99 TOX145-RTL-9R03253-M, Dayl, 5ag/kg, axt 10/13/99 TOXl5-RBS10229-250ppb-l, RWW MaOH Blank TOX14 5-RBS10229-H2O Blk-1, RMW TOX1I5-RBS10229-Sarua Blk-1, BMW TOX1I5-RBS10229-lppb-l, RWW TQX1I5-RS1Q229-Sppfe-1, BMW TOX145-RB510229-10ppb-l, BMW TOX145-RBS10229-25ppb-l, BMW TOX1I5-RBS10229-50ppb-l, RMW TQX145-BBS10229-100ppb-l, BMW TOX14S-RBS10229-2S0ppb-l, BMW TOX145-RBS10229-500ppb-l, RMW TOX145-RBS10229-750ppb-l, RMW TOXUS-BBSlOZ29-10QQppb-i, BMW Jtd C o w 0.99 4.93 9.76 24.80 19.30 97.60 248.00 493.00 735.00 976.00 248.00 248.00 248.00 248.00 248.00 0.99 4.93 9.76 24.80 <9.30 97.60 240.00 493.00 735.00 976.00 KT 6.822 6.793 6.821 6.825 6.818 6.813 6.826 6.815 6.809 6.817 6.811 6.806 6.807 6.809 6.844 6.813 6.811 6.822 6.820 6.818 6.821 6.820 6.811 6.818 6.815 6.808 6.811 6.814 7.100 6.811 6.806 6.810 6.822 6.810 6.818 6.839 6.811 6.019 6.810 6.821 6.815 6.810 7.173 6.808 6.796 6.808 6.823 6.006 6.814 6.791 6.807 6.811 6.815 6.799 6.815 6.806 6.826 6. 812 6.812 A rm 557 315 5022 609 1615 6515 7039 1292 21414 38054 774 74 125236 189194 232549 362 3894 4119 4255 5144 5636 79666 270 3172 4590 4364 4614 3782 77S81 150 37594 46851 42376 36393 40408 80830 181 28217 28068 36897 35914 31360 82686 79 8814 5855 87005 225 5847 5385 2075 7285 8322 15843 29105 56970 117936 203783 306442 374817 Cone, (ppt) flags 0.00 bd 0.00 bb 0.00 MM 0.00 MM 0.00 MMX 0.00 MMX 0.00 MMX 2.95 tt 39.07 bb 109.91 MM 277.72 MM 481.04 bb 753.30 bb 937.86 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 287.05 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 0.00 bb 278.17 bb 0.00 bb 107.95 bb 147.35 bb 128.31 bb 102.84 bb 119.93 bb 292.00 bb 0.00 bb 68.03 bb 67.39 bb 104.98 bb 100.80 bb 81.41 bb 299.90 bb 0.00 bb 0.00 bb 0.00 bb 318.29 KM 0.00 db 0.00 bb 0.00 bb 0.00 bdX 0.00 bbX 0.00 bbX 15.35 bbX 71.81 bbX 190.13 bbX 449.96 bbX 815.41 bbX 1252.42 bbX 1543.49 bbX %Dav -100 -100 -100 -88 -21 13 12 -2 2 -4 \ \ \ \ 16 1 I / / 1 i ' li ) J j excioTA- i2 < k n K r t A e A L Y ConC- tAC 10 18 \ 21 / / 28 / // -100 -100 -100 -38 16 95 81 65 70 58 Davey 070799: goantitatad and prmtad by aahlO/28/99 000637 % V* Oj N 1 rt'r~'fNe>'?ssai i i n c* o O T2S'-72~2SS 1 1 III 1 ssssslll sssasssass I ' "sssa5 1 1 ^Sslsii U s M s s mS 8 888888 888888 888 s ESSSS3 S2SSSE X2S 3S325S2SSP 5 3 sBassH S S S S S S s s a a s ss2SS I s i i s i ! m m 2sg "83531| | | | & sssissssss r-r-i-'r-r-r-r-r-r-r- 3 3 s ss ss s SS3SSS sss S s s l s s s s s l r- r- r~r- r~r~ r- r- r* r- r- f' r- i--r** r-r-f-r-r-r-r-r-r-f J ssssssggss ' "s s s 5Ss5 g 03 a sg 3 IN gg SSSSSSSSSS NN 3 sssss sssss s s ss ss Hilf lll Hill HI** s2s2s2s22s s s s s s2S^ 2S*42S-t2ST*2S-* 55555 999 99 22? =$ 9 99 00 22 SssX I1 1 1 H, I I I f 11! K, *! s iili1 llliiilfiiiiiliiiiiilfiiliiliillilHIilililiilifi jas 5 i i m r t V u i m i t t W n i m i m m i m i m i m m m m m m n ll I i i! i ! ! "*'-" " 2 s s s 2 s s s 2 2 s ^ i 3 3 s a s s s s s s i s s s s f . s s s ; = ; s s i S 2 s s s s s : K s : W 00 fo o<> o o \ i ! } 3 3 3 I I Quantify Coapeund Swaaaxy Report Tez 145: Rat Sera and Liver, Day 1 F F i ! i 4T O O O CD CO C l gggggggggg g S g g g gggggggggg ? e lllIIIIll?lllII!l2IlilIISIls ~o OMMMMMPHHOHHOHHHOHHHHOOOHOOHH^OOOHHHHOHHHHHHOOOOHHHHHMOHHOO sssksssbbbbbgkssgsssbssgssssbcgsssbbkggkkkskgsssgsbkkgsgggg ssss^g s;g II KgwS5cl c oKSSSS S iiiif  a g------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------ Q uantify C a lib ratio n M p e rt fo x 145: R at Sara and L iv a r, Day 1 & 4 t Mgm l 000640 Quantify Calibration Report Toz 145: Rat Sara and Livor, Day 1 & 4 * Pag 2 000641 Quantify Calibration Kapert Tor 143: Bat Sra and Livas, Day 1 6 4 * Pag 3 000642 Method Report Method fila : L u t modifiad: Compound : Printed: C:\KASSLYNX\Davay070799.PftO\MathOB\102799b.lb Thu Oct 29 08:57:32 1999 1: POAA (fune 1) Thu Oct 29 12:41:03 1999 Ccapound Nama: Intarnal Raf.: Quantify Traca: Cone. of Standards: Usar RF Valua: Usar Paak Factor: Intagrata Window Factor: Chromatogram mass window: POAA (fune 1) [Mona] TIC Cone. A 1.000000, Oisablad 1.000000 2.000 l.OOOODa Ratantion Tima (mins): Ralativa Ratantion Tiaa: RT Rafaranca: Tina Window (mins): Paak Salaction: 6.842, Snablad 0.000, Oisablad [Nona] 0.414 Naaraat Rasponsa Typa: Rasponsa: Extamal Araas Polynomial Typa: Point of Origin: Fit Waighting: Axis Transformation: Linaar Exeluda 1/X Nona Units: Paak-to-paak aaplituda: 492 Smoothing: Window siza (scans): Nuabar of smooths: Smoothing mathod: Disablad 1 1 Savitzky Golay Join vallay thrashold: Reduca paak tailing: Raisa basalina maximum: 5.00 50.00 10.00 Draw vartical thrashold: Datact shouldars: Shouldar thrashold: 25.00 Disablad 5.00 Ralativa haight: Absoluta haight: Ralativa araa: Absoluta araa: 1.50, Disablad 0.00, Disablad 2.00, Bnablad 0.00, Disablad -r Paga 1 000643 Method Report Method fila: Last modified: Coapoufd: Printad: C:\MA55LYNX\Davey070799.PRO\MethDB\l02799b.mdb Thu Oct 28 08:57:32 1999 2: 980 (fune 21 Thu Oct 28 12:41:03 1999 Coopound Nana: Zntarnal Raf.: Quantify Traca: Cone, of Standards: Usar Rf Valua: Usar Peak Factor: Intagrata Windew Factor: Chromatogram aass window: 980 (fune 2) (Nona] TIC Cooc. A 1.000000, Disablad 1.000000 2.000 l.QQOQOa Ratantion Tima (mins): Relative Ratantion Tioa: RT Rafaranca: Tima Window (mins): Peak Salaction: 7.620, Knablad 0.000, Disablad (Nona] 0.359 Xaarast Rasponsa Typa: Rasponsa: External Areas Polynomial Typa: Point of Origin: Fit Weighting: Axis Transformation: Linear Exclude 1/X Nona Units: Paak-to-peak amplitude: 444 Smoothing: Window size (scans): Number of smooths: Smoothing method: Disablad 1 1 Savitzky Colay Join valley threshold: Reduce peak tailing: Raisa baseline maximum: 5.00 50.00 10.00 Draw vertical threshold: Detect shoulders: Shoulder threshold: 25.00 Disabled 5.00 Relative height: Absolute height: Relative area: Absolute area: 1.50, Disabled 0.00, Disablad 2.00, Enabled 0.00, Disablad Paga 2 000644 Method Report Method file: Last modified: Compound: Printed: C:\HASSLTNX\Davey070799.PRO\MethDBU02799b.mdb Thu Oct 28 08:S7:32 1999 3: surr (func 3) Thu Oct 28 12:81:03 1999 Ccnpound N u : Internai Rai.: Quantify Traa: Cne, of Standards: User RF Valu#: User Peak Factor: Integrate Hindou Factor: Chroautoraa mass uindou: surr (func 3) {None] TIC Fixed 1.000000, Disabled 1.000000 2.000 l.OOOODa Ratantion Time (ins): Relative Rtention Time: RT Reference: Tiae Hindou (ins) : Peak Slection: .820, Enabled 0.000, Disabled (None] 0.2S Nearest Response Type: Response: External Areas Polyncadal Type: Point of Origin: Fit Heighting: Axis Transformation: Linear Exclude 1/X None Units: Peak-to-peak aaplituda: 629 Smoothing: Window size (scans): Number of smooths: Smoothing method: Disabled 1 1 Savitsky Golay Join valley threshold: Reduce peak tailing: Raise baseline aaxiaum: 5.00 SO.00 10.00 Draw vertical threshold: Detect shoulders: Shoulder threshold: 2S.00 Disabled S.OO Relative height: Absolute height: Relative area: Absolute area: 1.S0, Disabled 0.00, Disabled 2.00, Enabled 0.00, Disabled Page 3 00064S DAVEY 070799: FACT Equipment Log 99077 Quattro Ultima: #9261QB PAGE DATE: 10/27/99 ANALYST:mmh STUDY NUMBER: Toxl45: Matrix: Rat Sera& Liver DESCRIPTION: POAA& 980 FACT Mcthod:ETS 8-5.1 & 8-7.0 Injection volume: 5 uL Cycle time- 10 min Electrode: Z-Sorav Mobile Phase: (A12.0 mM NH4CH3CQ2 (BIMeOH_____ TN-A- or stndrd number (A) 99085-11-3_______ B1tn-a-2945 Prepared (date/by): (A) 10/23/99 sah ffil 10/23/99 sah Expires: (A) 04/00_____________ (B1 04/00 Store at room temp? 0 or N Other Guard column: None_________________ Part number: na________ Lot number: na Analytical column: Keystone Betasil_________________________________ Size: 2 x 50 mm_______________ Tyne: C18__________ Sphere size: 5 um______ Part number 055-701-2_________ Lot number: P9E11 Serial number: 0591825Z Analytical parameters: Drying gas (L/hrl: 487 ESI nebulizing gas (L/hr)_10__ Sheath gas (L/hrl 0 LC Flow rate: 300 uL/min. Back pressure: 82 bar HPLC solvent gradient: 10min-10-95 T i m ? (m in j ______ n o.oo______ 2 1 1.00___________ 31 5.50________ 4 7.50_________ 51 8.00_________ JM. 100 100 910 95.0 1M 000646 Tuning Method Report Page 1 Method: C:\MASSLXWX\DAVEY BACKUP AUG99\DAVEY-RATS.PRO\ACQUDB\PFOS-4 Printed: Wed Oct 27 14:31:21 1999 SOURCE ( ESP- ) Capillary(kV) Cone Hexapole 1 Aperture 1 Hexapole 2 Source Block Temp. Desolvation Temp. Set Rdbk 3.15 10 0.0 0.0 0.0 150 250 -3.07 -11 148 249 Pressures Analyser Vacuum Gas Cell Rdbk OFF 4.3e-3 Analyser LM Res 1 HM Res 1 IEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 IEnergy 2 Multiplier Gas Flows Cone Gas Desolvation Set Rdbk 14.5 14.5 1.0 -2 2 1 12.0 12.0 1.0 650 -3 2 0 -646 Rdbk 57.8 484.8 000647 S e a m i n g Method Wapact Method: C: \MkJSLYKX\aAVSr070799.PRO\ACQUDBMaMZM-POAA-980-ZS Last Modifiad: Mod Oct 27 14:19:01 1990 Printed: Wed Oct 27 14:32:05 1999 Solvent Delay ( nina ) : 0.00 function : 1 M M of 1 Mass Pair ( ESP- ) Intar Channel Delay < Secs ) : Span ( Daltons ) : Start Tina ( Mins ) : End Tiae ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell {Secs) Coll Energy <eV) Cone ( V 1 413.00 169.00 0.30 30 15 Ptswtien : 2 M M of 1 Mass Pair ( ESP- > Inter Channel Delay ( Secs > : Span ( Daltons ) : Start Tine ( Mins ) : End Tiae < Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) Coll Energy (eV) Cone ( V 1 960.00 78.00 0.30 60 60 function : 3 M M of 1 Maaa Pair ( ESP- ) Inter Channel Deley < Secs ) : Span ( Daltons ) : Start Tiaa ( Mins ) : End Tiae ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) Coll Energy <eV) Cone ( V 1 427.00 80.00 0.30 40 60 yyyQ x, / Z r S > 'T-^y Paga 1 00064S Method Report Method File: Last Modified: Printed: ' Page 1 C :\MASSLYNX\DAVEY070799.PRO\ACQUDB\10min Wednesday, October 27, 1999 14:25:05 Wednesday, October 27, 1999 14:25:31 HP1100 LC Pump Initial Conditions Solvents A% B% C% D% 90.0 10.0 0.0 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 0.300 10.0 0 400 30.0 30.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 5 entries which are : Time 0.00 1.00 5.50 7.50 8.00 A% 90.0 90.0 5.0 5.0 90.0 B% 10.0 10.0 95.0 95.0 10.0 C% 0.0 0.0 0.0 0.0 0.0 D% 0.0 0.0 0.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 HP1100 LC Pump External Event Timetable The Timetable contains 3 entries which are : Time Initial 0.00 0.10 Column Switch Contactl Off Off Off On Off Off Contact2 Off On Off Contact3 Off Off Off Contact4 Off On Off HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (ul/min) Draw Position (mm) Stop Time (mins) Injection Volume(ul) Vial Number 200.0 200 0.00 9.00 10.0 12 000649 Masslynx - Sample List Sample Ust: C:\MASSLYNX\Davey070799.PRO\SampleDB\102799b.SPL Printed: W ed Oct 27 14:34:05 1999 F ile N am e Pile Text 1 102799013 M eO H Blank 2 102799014 M eO H Blank 3 102799015 TO X145-R B S 10229-H 2O Blk-1, R W W 4 102799016 TO X145-R B S10229-Serum Blk-1, R W W 5 102799017 TOX145-RBS10229-1ppb-1, R W W 6 102799018 TOX145-RBS10229-5ppb-1, R W W 7 102799019 TOX145-RBS10229-10ppb-1, R W W 8 102799020 TOX145-RBS10229-25ppb-1, R W W 9 102799021 TOX145-RBS10229-50ppb-1, R W W 10 102799022 T OX145-RBS10229-100ppb-1, R W W 11 102799023 T 0 X 1 4 5 -R B S 10229-250p pb -1. R W W 12 102799024 TO X145-RBS10229-500ppb-1, R W W 13 102799025 TOX145-RBS10229-750ppb-1, R W W 14 102799026 TOX145-RBS10229-1000ppb-1, R W W 15 102799027 M eO H Blank 16 102799028 TO X 145-R T S -9R 03230M . Day1, control ,-ext10/19/99 17 102799029 TO X145-R TS-9R 03231M , Day1, control,-ext10/19/99 18 102799030 TO X 145-R TS -9R 03232M , Day1, control,-ext10/19/99 19 102799031 T 0 X 1 45-R TS -9R 03233M , Day1, control,-ext10/19/99 20 102799032 T OX145-RTS-9R03234M , Day1, control.-ext10/19/99 21 102799033 T O X 145-R B S 10229-250ppb -1, R W W 22 102799034 M eO H Blank 23 102799035 T 0 X 1 45-R TS-9R 03235M , Day4, control,-ext10/19/99 24 102799036 TO X145-RTS-9R03236M , Day4, control,-ext10/19/99 25 102799037 T 0 X 1 45-R TS -9R 03237M , Day4, control,-ext10/19/99 26 102799038 TO X145-R TS-9R 03238M , Day4, control,-ext10/19/99 27 102799039 TO X145-R TS-9R 03239M , Day4, control,-ext10/19/99 28 102799040 T 0 X 1 45-R B S 10229-250ppb-1, R W W 29 102799041 M eO H Blank 30 102799042 TO X145-R TS-9R 03245M , Day1, 5mg/kg, D50-ext10/19/99 31 102799043 T O X 1 45-R T S -9R 032 46M , Day1, 5m g/kg, D 5 0 -ext10/1 9/99 32 102799044 TO X145-R TS-9R 03247M , Day1, 5mg/kg, D 50-ext10/19/99 33 102799045 TO X145-R TS-9R 03248M , Day1, 5mg/kg, D50-ext10/19/99 34 102799046 T 0 X 1 45-R TS -9R 03249M , Day1, 5mg/kg, D50-ext10/19/99 35 102799047 TOX145-RBS10229-250ppb-1, R W W 36 102799048 M eO H Blank 37 102799049 T 0X 1 45-RTS-9R03250M , Day4, 5m g/ka ext10/19/99 38 102799050 T 0 X 1 45-R TS-9R 03251M , Day4, 5mg/kg, ext10/19/99 39 102799051 TO X145-R TS-9R 03252M , Day4, 5mg/kg, ext10/19/99 40 102799052 T 0 X 1 45-R TS -9R 03254-1M, Day4, 5mg/kg, ext 10/19/99 41 102799053 T 0 X 1 4 5 -R T S -9R 0 325 4-2M , Day4, 5m g/kg, ext 10 /19/9 9 42 102799054 T O X 1 4 5 -R B S 102 29-250p pb -1, R W W 43 102799055 M eO H Blank 44 102799056 TO X145-R TL-9R 03247-M , Day1, 5mg/kg. ext 10/13/99 45 102799057 T OX145-RTL-9R03253-M , Day4, 5m g/ka ext 10/13/99 46 102799058 T 0 X 1 4 5 - R B S 102 29-250p pb -1, R W W 47 102799059 M eO H Blank 48 102799060 TO X 145-R B S 10229-H 2O Blk-1, R W W 49 102799061 T 0 X 1 4 5 -R B S 1 0 2 2 9 -S e ru m Blk-1, R W W 50 102799062 TO X145-RBS10229-1 ppb-1, R W W 51 102799063 TO X 145-R B S 102 29-5p p b -1, R W W 52 102799064 T 0 X 1 45-R B S10229-10ppb-1, R W W 53 102799065 T O X 1 4 5 -R B S 10229-25pp b-1, R W W 54 102799066 TOX145-RBS10229-50ppb-1, R W W 55 102799067 TOX145-RBS10229-100ppb-1, R W W 56 102799068 TOX145-RBS10229-250ppb-1, R W W 57 102799069 TOX145-RBS10229-500ppb-1, R W W 58 102799070 TO X145-RBS10229-750ppb-1, R W W Page 1 Page Position: (1, 1) 00650 Masslynx - Sample List Sample Ust: C:\MASSLYNX\Davey070799.PRO\SampleDB\102799b.SPL Printed: Wed Oct 27 14:34:05 1999 Page 2 Page Position- (2 1) MS File Inlet File Bottle Inject Volum e Sam ple Type C on e A 1 10MI N-POAA-980-1S 10m in-10-95f 91 2 10MI N -P O A A -980-IS 10m in-10-95f 91 3 10MI N-POAA-980-IS 10min-10-95f 1 4 10MIN-POAA-980-IS 10min-10-95f 2 5 10MIN-POAA-980-IS 10min-10-95f 3 6 10M I N -P O A A -980-1S 10m in-10-95f 3 7 10MIN-POAA-980-IS 10min-10-95f 4 8 10M I N -PO A A -980-IS 10m in-10-95f 5 9 10MI N-POAA-980-IS 10min-10-95f 6 10 10MI N-POAA-980-IS 10min-10-95f 7 11 10MI N-POAA-980-1S 10m in-10-95f 8 12 10MI N-POAA-980-IS 10min-10-95f 9 13 10MI N-POAA-980-IS 10min-10-95f 10 14 10MI N -PO A A -980-IS 10m in-10-95f 11 15 10MIN-POAA-980-IS 10min-10-95f 92 16 10MIN-POAA-980-IS 10min-10-95f 12 17 10M I N-POAA-980-1S 10m in-10-95f 13 18 10MI N-POAA-980-1S 10mir*-10-95f 14 19 10MI N-POAA-980-1S 10mir-10-95f 15 20 10MI N-POAA-980-1S 10min-10-95f 16 21 10M IN -P O A A -980-IS 10m in-10-95f 8 22 10MI N-POAA-980-1S 10min-10-95f 92 23 10MI N-POAA-980-IS 10min-10-95f 17 24 10MI N-POAA-980-1S 10min-10-95f 18 25 10MI N-POAA-9804S 10min-10-95f 19 26 10MIN-POAA-980-IS 10min-10-95f 20 27 10MI N -PO A A -980-IS 10m in-10-95f 21 28 10MIN-POAA-98O-IS 10min-10-95f 8 29 10MIN-POAA-980-IS 10min-10-95f 93 30 10M I N-POAA-980-1S 10m in-10-95f 22 31 10MI N-POAA-980-1S 10m in-10-95f 23 32 10MI N-POAA-980-1S 10min-10-95f 24 33 10MI N-POAA-980-1S 10min-10-95f 25 34 10MI N-POAA-980-1S 10min-10-95f 26 35 10MI N-POAA-980-1S 10min-10-95f 8 36 10MI N-POAA-980-1S 10min-10-95f 93 37 10MI N-POAA-980-1S 10min-10-95f 27 38 10MI N-POAA-980-1S 10min-10-95f 28 39 10MIN-POAA-980-IS 10min-10-95f 29 40 10MIN-POAA-980-IS 10min-10-95f 30 41 10M IN -P O A A -980-IS 10mir-10-95f 31 42 10MI N-POAA-980-1S 10min-10-95f 8 43 10MI N-POAA-980-1S 10min-10-95f 94 44 10MI N-POAA-980-1S 10m in-10-95f 41 45 10MI N-POAA-980-1S 10m in-10-95f 42 46 10MI N-POAA-980-1S 10m in-10-95f 8 47 10MI N-POAA-980-1S 10min-10-95f 94 48 10MIN-POAA-980-IS 10min-10-951 1 49 10MI N-POAA-980-1S 10min-10-95f 2 50 10MI N-POAA-980-1S 10rni n-10-951 3 51 10MI N-POAA-980-1S 10m in-10-95f 3 52 10MI N-POAA-980-1S 10min-10-951 4 53 10MI N-POAA-980-1S 10min-10-951 5 54 10MIN-POAA-980-IS 10min-10-951 6 55 10MIN-POAA-980-IS 10min-10-951 7 56 10MINI-POA A -980-IS 10min-10-951 8 57 10MIN-POAA-980-IS 10min-10-95f 9 58 10MIN-POAA-980-IS 10min-10-95f 10 10 __ 10 __ 10 __ 10 -- 2 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 __ 10 __ 10 __ 10 __ 10 __ 10 10 __ 10 10 __ 10 10 _ 10 -- 10 __ 10 10 __ 10 10 __ 10 __ 10 __ 10 10 Q C 10 _ 10 10 10 __ _ 10 10 10 QC 10 10 -- 10 __ 10 Q C 10 10 10 __ 2 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard _ -- __ __ __ __ __ __ __ __ __ __ __ __ __ -- _ _ __ _ __ _ _ __ _ ,,,, - , -- .. -- -- mmm -- 006Sl M asslynx - S am p le List Sample Ust: C:\MASSLYNXMDavey070799.PRO\SampleDB\102799b.SPL Printed: Wed Oct 27 14:34:05 1999 File N am e File T ext 59 102799071 TO X145-RBS10229-1000ppb-1, R W W Page Position: (1 2) 000652 Masslynx - Sample List Sample List: C:\MASSLYNJQDavey07Q799.PRO\SampleDBV102799b.SPL Printed: Wed Oct 27 14:34:05 1999 sy d fy / / 'JT-97 Page 5 Page Position' (2 2) MS File Inlet File Bottle Inject Volume Sample Type Cone A 59 10MI N-POAA-980-1S 10m in-10-95f 11 10 Standard 0006S3 Dale Dala Analyse &S FACT: DATA REVIEW SU M M A R Y FO RM Data ReviewSign-OfT A nalyst Review ,, Nam / Dale: 3 < "fertf l' 2 w- ulfril'K FACT Study *: "My' N S Matnx/Timepoinu: n o s* ,(/1/ T echnical Review A t / , . / - r * / / 3 / f JkC ff Name / Date: , A Sample Lia: Set-up Analysis Date/Anolyst: Instrument: f / o j f f . ___________________________________________ 3* Ssm>otrtfj Q uality A ssu ran ce Review Name / D ate:_____________ Data Entry:. CAC nloslw Comments / Justifications: _ _ _ _ _ _ _ A nalyte: CHI') Acceptable Linear Rana: A/A LOO: m RA2: na, Calibration Cheeks: AM MS/MSD: Data Ststus 0 MA ajA Analyte: 7FoS (CH*') Acceptable Linear Range: LOQ:. l i f l L R-2: ? t ? 7 ? Extraction Blank: /A 4 M atrix Blank: fJA IAC ulosh"! Extracted Blank: /&C -Moti O. M atrix Blank: /* S S J M , ^ ^ 0Jil}ltJ/A . iinx. mas, n d ktui Jar TkAA. JhM. as us*Jtt./ art. fe u d 's Q * J V ejcdi**. ~h> D r J u . - ~ 3 5 s ^ H / x s f o ___________________________ LhJ ]* !* ( D a t'd . kMs k J ~2-* h telty "M*. 4l*. eii'/yd.c^/>*J * & t JL# J> a td iM S eJC i/uJec/ 4rtm . '/ t tiu fa - 4o J ts ^ u J ty a A kUJatL -fta j hjUM L u * . / 7 7_ ^ ; ,7, tdkckJ j hdckyoiuu:/ jm 0 / 7 & - J lmm LJih . -'Jstfof/Y_______________________ hJSs e x c l u d e d Calibration Checks: 0 K ~ E i* a e /vam . - 7 % 9 ~ /? / pw ich` h * t r r >*y 'u fpua.y' S^ISD :------------ K - o n e U & W a - l L T / d i l l r t p i - W ^ fgjutt CLPayePt t a - h c/aJa. . Data Sums: _ c W d aempWs n a A l .\D i L U r . Analyte: Acceptable Linear Range: m ^k. ____ 33&k . // Extracted Blank: ffS S Si 4M atrix Blank: i f aa L t i Calibration Cheeks: 0 - 0 i n j e fv'iVL ~ '/o ~/3% M S.M SD:. D ita Satus: _ 0 K _ ________________ ( A l l l l o s h tA06 \tk lW 'fc Irfan 4M - * ? f ? ____________________ OOGS4 FACT: DATA REVIEW SUM MARY FORM Date: Data Analyst: J#S FACT Study*: Matnx/Timepoints: 7*.U s ,. /. Sera - 7)*u 9 a o S t e u d S a w * ! - mt fh n 9 Sample Lin: ttdffu Set-up Analysis Date/Analyst Js Data Review Sign-Off Analyst Review ., Name / Date: J A s 'w o S n _________ T echnical Review Nam e/ Date: _ _ _ _ J S i ^ U P M - Q uality A ssurance Review N am e/D ate:_____________ D ata E n try :. u c 11losing Com m ents / Ju stificatio n s: lAC- u lo im (AC i i k d V i 000655 ! 0 wWeH <0 j s(* & 1 8 s & Ht 8 9S9000 kuKJHOVMB'JC JMMUUMU OOOOOOc 3 OOOOOOOOOOOOOOOQ0 OOOOOOOOC d o o o o o o o e o l oooooooooooooooooooooooooooooooooooooooooooooo JMOtf B-JOlU HOISIBslM^WKIHOUa>J(MXwKIHOlCDNl9lUI^UKIH 83888888883818888883883188888388888888883881111 I DVtKUtUIVM/IVRUIUtUIMMW^WUiUlVIUlSSIil gM JgMgMgMgHgJgJgW gM J Mg g EW g mI gM3i33Img3 3 3IJ I3a 3I WEWg gMgUgUgWgW gW Wg WgU3UgHgUE E E * ooooooooooo o uuuwuuwuuuwu enM u..o..o.. wo 9o$ -ye*-e*-JovMo9W l ^^lMHVKlHlil ev ovteoino H ooDooggflQMO O"-- -`---i---T-- -w 'hh te x >r S??? ?? S-"-s55 m BHB B UM -jfiB nnnnnnnnr iafafaiafafaiaiajs * | f* K H H H K 5^55 55 555 .^ssss- . s EEE?"-'*. Ih h * i ku w t <X*vSI*HHN `-p so y W. y jj i ^S5 # 55555 23s laialaiuas Mf i ?m i n* n * iy r j s j !? i <t f ! !|!|! O 0S0H " "B"B ll HKHIt ta t* v T! ? m cOH H8*" SM ^ OM* ` 5 fi j m cji-o a u ju i w e g p g > HOH o esO jgg g g g g g g g g g <H H H H H O H Jtom MUfOcWMHUWflHH Oh- OoVt jgg>4gggg m s g i g g g m g g gSggg SSgggS g g jg g g g jg g g ? OQOOOOQQOH Oh OHHOOO OOOt-*OO ig t*eso otos o u H i t o o M M w u o es wow m o * t * g o g g jo eauiftgogg !C\ * to""* i5 ^ M^ o <J - ! I -T T saasra 5 n7 s^-sss-ss fl i i i i t i i ggggggSS5S3333S353gggSgggS35SSSS5SgggSS?3i;i:33S fi clS lS iiS ssS sssS i = S ~ = i = g | | S | 3 = - = | = = S | | g s 3 | | = 3 = SSS 3 s j | g | | S S iM 3 !S 3 M 3 3 9 3 :3 n U M 3 S s j:M M M M ^ 000657 Quantify Compound l u n u y Rupert TOX145-rat sur*, day 29 dene end control- ext. 11/3/9 Maple List: C:\UJL99LTUX\eoup0201.pro\*e^leDPM10tf*e U l C Modified: Rri Nov OS 0:30:ll 199 Method: C:\HX88LtMX\aoup0201f9.proYMethinui0499a Lent Modified: rri Mov 09 08:29:44 1999 Job Cede: mated: Fri Nov OS 04:33:31 199 cexpound 3: rroaa <Ch3) Mane 1 110499001 3 110499002 3 110499003 4 110499004 S 110499005 6 110499006 7 110499007 a 110499008 9 110499009 10 110499010 11 110499011 12 110499012 13 110499013 14 110499014 IS 110499015 16 110499016 17 110499017 18 110499018 19 110499019 20 110499020 21 110499021 22 110499022 23 110499023 24 110499024 2S 110499025 26 110499026 27 110499027 28 110499028 29 110499029 30 110499030 31 110499031 32 110499032 33 110499033 34 110499034 35 110499035 36 110499036 37 110499037 3B 110499038 39 110499039 40 110499040 41 110499041 42 110499042 43 110499043 44 110499044 45 110499045 46 110499046 Ranpleliet Text Type HeOK ileal KeOK Blank MeOK Blank TOX145-MS11039-82O Blk-9. ext. 11/3/99 MCH TOX145-RBS11039-Sera Blk-9. ext. 11/3/99 MCH TOX145-RTSUO 39-Sera Blk-9. ext. 11/3/99 MCH TOX145-RBS11039-5ppb-9. ext. 11/3/99 MCB Standard TOX145-RBS11Q39-10ppb-9. ext. 11/3/99 MCH Standard TOX14S-RBS11039-25ppb-9. ext. 11/3/99 MCB Standard TOX145-RBS11039-5Oppb-9. ext. 11/3/99 MCH Standard TOX145-XBSll039-100ppb-9. ext. 11/3/99 MCH Standard TOX145-KBSU039-250ppb-9. ext. 11/3/99 MCH Standard TCXL145-RB511039-500ppb-9, ext. 11/3/99 MCH Standard TOX145-RBS11039-750ppb-9. ext. 11/3/99 MCB Standard TOX145-*lSll039-1000ppb-9. ext. 11/3/99 MCH Standard MeOH Blank TOX145-XTS11039-250ppb-MS9, ext. 11/3/99 MCH TOX14S-XTS11039-250ppb-MSD10. ext. 11/3/99 MCH TOX145-RTS-9R03240M-0-Day 29. ext. 11/3/99 MCH TOX145-*TS-9*03241M-0-Dey 2, ext. 11/3/99 MCH TOX145-RTS-9H03242M-O-Dey 29, ext. 11/3/99 MCH TCX145-R3S11039-250ppb-CCV9, ext. 11/3/99 MCH QC MeOH Blank TOX145-RTS-01241M-0-Dey 29, ext. 11/3/99 MCB TOX145-RTS-9X03243M-0-Dey 29, ext. 11/3/99 MCH TOX14S-ltTS-9RO3255M-Sn0/k0-Dey29, ext. 11/3/99 MCH TTOOXX114455--RRTTSS--99RR0033225567MM--SSaaag//kkag~-DDeayy2299,, ext. ext. 11/3/99 11/3/99 MCH MCH TOX145-RBS11039-2S0ppb-CCV10. ext. 11/3/99 MCH QC MeOH Bleak TQX145-RTS-9RQ32S8K-5eM/kQ-Dey29, ext. 11/1/99 MCH TOX145-RTS-9B032S9H-5aa/kg-Dey29, ext. 11/3/99 MCH TOX145-RBS11039-250ppb-CCV9, ext. 11/3/99 MCH OC MeOH Blank TOX14S-XBS11039-K2O Blk-9. ext. 11/3/99 MCH TOX145-RSS11039-Sera Blk-9, ext. 11/3/99 MCH TOX145-RTS11039-Sera Blk-9. ext. 11/3/99 MCH TOX145-RBSU039-5ppb-9. ext. 11/3/99 MCB Standard TOX145-RB511039-10ppb-9, ext. 11/1/99 MCH Standard TOX145-RS511039-25ppb-9, ext. 11/1/99 MCH Standard TOX145-RBS11039-50ppb-9. ext. 11/3/99 MCH Standard 7OX145-RB511019-100ppb-9. ext. 11/3/99 MCH Standard TOX145-RB511039-2S0ppb-9. ext. 11/1/99 MCH Standard TOX145-RB51103-500ppb-9. ext. 11/1/99 MCH Standard TOX45-RBS11039-7$0ppb-9. et. 11/1/99 MCH Standard TOX145-RBS11039-10Q0ppb-9, ext. 11/3/99 MCH Standard Std Cone 4.93 9.77 24.80 49.30 97.70 248.00 493.00 716.00 977.00 24.00 248.00 248.00 4.93 9.77 24.80 49.30 97.70 248.00 493.00 736.00 977.00 XT 7.805 7.815 7.809 7.769 7.805 7.871 7.850 7.828 7.875 7.857 7.816 7.853 7.875 7.837 7.835 7.860 7.832 7.808 7.855 7.851 7.847 7.811 7.872 7.174 7.859 7.875 7.926 7.874 7.811 7.878 7.111 7.856 7.812 7.918 7.873 7.948 7.876 7.810 7.808 7.918 7.876 7.872 7.945 7.809 7.879 7.861 krea A a o s 236 MM 84Q MX 522 MM 363 Ml 409 MC 544 bb 1849 db 3250 db 7052 dd 13252 db 2S632 MM 66768 MM 125323 Ml 187764 Ml 241229 Ml 1516 Ml 61127 Ml 60819 Ml 674 Ml 600 Ml 417 KM 58654 Ml 541 KM 370 Ml 323 MM 677 db 939 Ml 911 db 55323 MM 286 MC 929 MC 1875 db 51678 MC 360 Ml 229 Mt 240 MM 283 db 1629 MM 2912 NM 6272 MM 11757 MH 24931 MC 60206 MM 122823 Ml 172738 Ml 230763 MC eene. MOev 0.00 0.80 0.00 0.00 0.00 0.00 4.91 -0 10.61 9 26.09 5 51.32 4 113.91 17 269.12 9 507.43 3 761.56 3 979.16 0 3.55 246.16 245.19 0.13 0.00 \ \ \ 0.00 236.10 0.00 0.00 "5 /J r 0.00 7 0.14 1.20 \ 1.09 222.54 0.00 1.16 5.01 215.85 -10 /I ///-13 0.00 0.00 0.00 0.00 4.01 -19 9.23 -5 22.91 -8 45.23 -8 98.85 1 242.42 -2 497.26 1 700.41 -5 936.56 1. .j wc ii/a s/tt 1 { ! i i Soup 030199: Quantitated and printed by lea on 11/09/99 000658 Quantify Compound l U M u y Mport TOX145-rae M r t , day 29 don and control 11/3/99 I d anpl* bla: c:\MMiLVMXNaobp020199.proVflaaplaDB\U0499a baa Mdlflad: rrl Mo t OS 04:30:1 1999 Nothod: C:\KRJ8LyMX\MmpO2O199.pro\MaehSft\110499a baa aodlflad: rrl Mov OS 04:39:44 1999 Job Coda: rrlnad: rrl Mo t OS 04:S3:31 1999 Compound 4: urr (Ch4) aaa 1 110499001 2 110499002 3 110499003 4 110499004 5 110499005 6 110499006 7 110499007 8 110499008 9 110499009 10 110499010 11 110499011 12 110499012 13 110499013 14 110499014 IS 110499015 16 110499016 17 110499017 IS 110499018 19 110499019 20 110499020 21 110499021 22 110499022 23 110499023 24 110499024 25 110499025 26 110499026 27 110499027 28 110499028 2 110499029 30 110499030 31 110499031 32 110499032 33 110499033 34 110499034 35 110499035 36 110499036 37 110499037 38 110499038 39 110499039 40 110499040 41 110499041 42 110499042 43 110499043 44 110499044 45 110499045 46 110499046 Baaplollae taat *ypa MaOH Blank MaOH Blank MaOH Blank TOX14S-RK11D39-K20 Blk-9, mxt. 11/3/99 MCH TOX145-RBSli039-Sra Blk-9, axt. 11/3/99 MCH TOX145-rrsll039-Sara Blk-9. axe. 11/3/99 MCH TOX145-RSSU039-Sppb-9. axt. 11/3/99 MCB Standard TOX14S-US11039-10ppb-9. ax. 11/3/99 MCH Standard TOX145-ftBS11039-2Sppb~9, mxt. 11/3/99 MCH Standard TOX145-US11039-50ppb-9, axt. 11/3/99 MCH Standard TOX14$-US11039-100ppb-9. axt. 11/3/99 MCH Standard TOX14S-RBS11039-250ppb-9, axt. 11/3/99 MCB Standard TOX14S-XBS11039-SOOppb-9. axt. 11/3/99 MCH Standard ?OXlS-MS11039-?S0ppb-9. axt. 11/3/99 MCB Standard TOX145-XBSll039*1000ppb-9, axt. 11/3/99 MCH Standard MaOH Blank tOX14S-*TS11039-250ppb-NS9. axt. 11/3/99 MCH TOX14S-RTS11039-250ppb-KSD10, axt. 11/3/99 MCH TOX14S-SETS-9X03240M-0-Day 29. axt. 11/3/99 MCH TOX145-XTS-9R03241M>0-Day 29. axt. 11/3/99 MCB TOX145-RTS-9R03242M-0-Dny 29, axt. 11/3/99 MCH TOX145-U11039-2S0ppb-CCV9. axt. 11/3/99 MCB QC MaOH Blank TOX145-RTS-9R03243M-0-Day 29. axt. 11/3/99 MCH TOX14S-ftTS-9R03243M-0-Day 29. axt. 11/3/99 MCH TOX145-RTS-9R032SSM-SMg/kg-Day29. axt. 11/3/99 MCB TOX14S-RTS-9R03256M-Sag/kg-Day29. ax. 11/3/99 MCH TOX14S-KTS-9R032S7M-Sag/kg-Day29, axt. 11/3/99 MCH TOX14S-RBSllQ39-230ppb-CCV10. axt. U/3/99 MCH QC MaOH Blank TOX145-RTS-9R032S8M-5aQ/kg-Day29, axt. 11/3/99 MCH TOX145-RTS-9R032S9M-5xg/kg-Day29. axt. 11/3/99 MCB TOX145-RBSll039-250ppb-CCV9, axt. 11/3/99 MCH QC MaOH Blank 7OX145-RBS11039-H2O Blk-9, axt. 11/3/99 MCH TOX145-RBS11039-Sara Blk-9, axt. 11/3/99 MCH T0X145-RTS11039-Sara Blk-9. axt. 11/3/99 MCH TOX145-RBSU039-Sppb-9. axt. 11/3/99 MCH Standard TOX14S-RB511039-10ppb-9. axt. 11/3/99 MCH Standard TOX145-RBS11039-2Sppb-9, axt. 11/3/99 MCH Standard TOX14S-RB11039-50ppb-9, axt. 11/3/99 MCH Standard TX14S-RBSll039-100ppb-9. axt. 11/3/99 MCH Standard TOX145-RBS11039-250ppb-9, axt. 11/3/99 MCH Standard TOX145-RBSll039-500ppb-9, axt. 11/3/99 MCH Standard TOX145-RBS11039-750ppb-9, axt. 11/3/99 MCH Standard TOX145-RBS11039-1000ppb-9, axt. 11/3/99 MCH Standard ted Cone 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 l.QQ 1.00 1.00 1.00 1.00 1.00 1.00 1.00 KT 7.075 7.085 7.058 7.097 7.122 7.123 7.123 7.105 7.128 7.168 7.121 7.130 7.106 7.131 7.106 7.077 7.125 7.146 7.143 7.126 7.167 7.167 7.128 7.124 7.129 7.122 7.080 7.102 7.105 7.100 7.163 7.122 7.154 7.191 7.124 7.102 7.144 7.080 7.099 7.127 7.126 7.105 7.130 At m riapa 14 MM Cone. HOOT 0.01 -99 2657 bb 2772 bb 2201 bb 2219 bb 2541 bd 2415 bb 2030 bb 2372 bb 2178 bb 2352 bb 2306 bb 2191 bb 10 bb 1907 bb 1730 bb 1490 bb 2231 bb 2377 bb 2260 bb il m 2212 bb 2451 bd 2005 bb 2380 bb 2507 bb 1986 bb 2213 bb 2002 bb 2025 bb 9 bb 1877 MX 2008 bb 1671 bb 1925 bb 2102 bd 2068 bb 1741 bb 2120 bb 2076 bd 2239 bb 2002 MM 1894 bb 1.23 23 1.29 29 1.02 2 1.03 3 1.18 18 1.12 12 0.94 -6 1.10 10 1.01 1 1.09 9 1.07 7 1.02 2 0.00 -100 0.89 -11 0.80 -20 0.69 -31 1.04 4 1.10 10 1.05 5 0.01 -99 1.03 3 1.14 14 0.93 -7 1.11 11 1.16 16 0.92 -8 1.03 3 0.93 -7 0.94 -6 0.00 -100 0.87 -13 0.93 -7 0.78 -22 0.89 -11 0.98 -2 0.96 -4 0.81 -19 0.98 -2 0.96 -4 1.04 4 0.93 -7 0.88 -12 oup 030199: Quaaiaad ad priaad by in* on 11/0S/99 000659 7* M__________________________________________________ __ ________________________________________________ 'V W /f? j. Quantify Calibration p o rt ___ TCX14S>rat atra, Cay 29 4oaa aad entrai- act. 11/3/99 m tae* 1 0006S0 Quantify Calibration fcaport TQXl4S>rae aora, day 29 doaa Ml control- met. 11/3/99 MCI M* 2 000661 Q u a t l f y Calibration Raport TOXllS-rat m m day 39 Co m and oontrel- ont. 31/3/99 m Mga 3 C''0SS2 fO U t S - r a t aara, day 21 dos oootrol- xt. 11/3/ MCI 000663 Method Report Natbod ila: Last modified: Compound: Printed: C:\XASSLYia\soup020199.pro\HathDS\110499a.mdb fri Nov 05 04:29:44 1999 1: POAA (Chi) fri Mow OS 04:54:56 1999 Compound Maaa: Intamal Ra.: Quantify Trace: Cone, of Standard: Uaer W Value: Usar faak Factor: Integrate window factor: Chromatogram aaaa window: FQAA (Chi) [Mona] TIC fixed 1.000000, oisabl 1.000000 2.000 1.00000a Retention Tima (aina): Relative Ratantion Tima: XT Rafaranca: Tima Window (aina}: faak Salaction: 7.167, enabled 0.000, Disabled (Monel 0.145 eareat Xaaponaa Typa: Raaponaa: External Areas Polynomial Typa: Point of Origin: fit Weighting-. Axis Transformation: Linear taelmde 1/X one Units: -- Peak-to-peak amplitude: 1 Smoothing: Window size (scans): number of smooths: Smoothing method: Bnabled 2 1 Join valley threshold: Reduce peak tailing: Raise baseline maximum: 30.00 200.00 5.00 Draw vertical threshold: Detect shoulders: Shoulder threshold: 90.00 Disabled 30.00 Ralativa height: Absolute height: Relative area: Absolute area: 1.50. Disabled 0.00, Disabled 2.00. Disabled 0.00. Disabled \ tJ 4 l f tag 1 C00664 Method Report Method Cila: Last noditied; Ceapound: Printed: C:\MASSLYWX\soup020199.proUtethDB\110499a.ndb Pri MOV 05 00:29:44 1999 2: PPOS <Ch2) Pri Mov 05 00:50:50 1999 Compound Maas: lacaraal Ref.: Quantify Traca: Coac. of Standards: User HI Valua: User Peak Factor: Integrate Window Factor; Chromatogram mass window: pros ( c h 2 ) (Mona] TIC Cone. A 1.000000, Disabled 1.000000 2.000 1.00000a Ratastion Time (mins) : Ralativa Rataatioo Time; RT Rafaranca: Time Window (mina) : Peak Salaction: 7.429, Enabled 0.000, Disabled [Mena] 0.447 nearest Raaponaa Typa: Raaponaa: Exta n a l Areas Polynomial Typa: Point of Origin: Pit Weighting: Axis Transformation: Linear heluda l/l Units; Peak-to-peak amplitude: 1 Smoothing: Window sise (scans): Number of smooths: Saoothing aatbod: Enabled 2 1 Join vallay thraahold: Raduea paak tailing: Raisa basalina a w i a a ; 30.00 200.00 5.00 Draw vartical thraahold: Dataet shouldars: Sbouldar threshold: 90.00 Disabled 30.00 Ralativa height; Absolute height: Ralativa area: Absolute area: 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled Mg* 2 ^00665 Nached Rtporc Method file: Last modified; Compound: Printed: C: \MASSLY10t\S<3Up020199 .pro\MathDB\110499s.mdb Pri Nov 05 04:29:44 1999 3: PPOSA <Ch3> Pri Nov 05 0C:SC:5< 1999 Compound Name: Internal Kef.: Quantify Trace: Cone, of Standards: Oaer XP Value: Oser Peak Factor: integrate Window Factor: Chromatogram mass window: PPOSA (Chi) [None] TIC come, a 1.000000. Disabled 1.000000 2.000 l.OOOODa Retention Time (mins): Relative Retention Time: RT Reference: Time Window {mins): Peak selection: 8.147. Enabled 0.000. Disabled [None) 0.55 Nearest Response Type: Response: External Areas Polynomial Type: Point of Origin: Pit Weighting: Axis Transformation: Linear Exclude 1/X Nome Units: -- Peak-to-peak amplitude: 11 Smoothing: Window sire (scans): Number of smooths: Smoothing method: Enabled 2 1 Join valley threshold: Reduce peak tailing: Raise baseline maximum: 30.00 200.00 5.00 Draw vertical threshold: Detect shoulders: Shoulder threshold: 90.00 Disabled 30.00 Relative height: Absolute height: Relativs arse: Absolute area: 1.50, Disabled 0.00, Oiaabled 2.00. Disabled 0.00, Disabled * Page 3 000666 Method Report Method file; Lest aodified: Compound: Printed: C:\KA5SLYNX\soup020199.pro\MethDE\110499a.ndb Fri Mov OS 06:29:44 1999 4s Surr (Chi) Pri Nov 05 06:56:56 1999 Compound NSM: Internal Ref.: Quantify Trace: Cone, of Standards: User RF* Value; User Peat Factor: Integrate Window factor: Chroauttograa (mass window: Surr (Chi) (None) TIC fixed 1.000000, Disabled 1.000000 2.000 l.OOOODa Retention Tiae (mins): Relative Retention Tiae: RT Reference: Tiae Window (nine) : Peak Selection: 7.211, Enabled 0.000, Disabled (Hone} 0.379 Nearest Response Type: Response: External Areas Polynoadal Type: Point of Origin: fit Weighting: Axis Transforoation: Linear Bxelude l/x Hone Units: Peak-to-peak aaplituda: SI Saoothing: Window size (scans): Nuaber of saooths: Saoothing nethod; Enabled 2 1 Join valley threshold: Reduce peak tailing: Raise baseline aaxisaae: 30.00 200.00 S.00 Draw vertical threshold: Detect shoulders: Shoulder threshold: 90.00 Oisabled 30.00 Relative height: Absolute height: Relative area: Absolute area: 1.50. Disabled 0.00. Disabled 2.00, Disabled 0.00, Disabled ' Pig 4 000667 Q uattro II, #6414E SOUP 020199: FACT Equipment Log 99092 PAGE 1/1 DATE: 11-04-99 ANALYST:ias STUDY NUMBER: TO X 145 MATRIX: rat sera DESCRIPTION: day 29- dose & control FACT Method: ETS-g-g.j Injection volume: 10 uL Cvcle time: 10 min. Electrode: Z-Sorav Mobile Phase: A12.0 mM NH4CH3C02 IBI MeOH TN-A- or stndrd number /A) 99085-11-15 CB) TN-A-2997 Prepared (date/by): (A ) 10/30/99 sah_______ (B ) 10/30/99 sah Expires: (A ) 04/00 (B) 2010 Store at room temp? Yj or N Other: G uard column: N<?h? Part number: na Lot number: na Analytical column: Keystone Bctasil tutu Part number: Q55-7Q1-2__ Lot number: P9E11 _ Serial number:0591804Z_______ Analytical parameters: Drying gas (TVhr): 350 ESI nebulizing gas (L/hr) 13 LC Flow rate: 300 uL/min . Back pressure: 65 bar Sheath gas (L/hr) 0 HPLC solvent gradient: 10min-10-95 1)0.00 2) 1.00 3) 5.50 4) 7.50 5) 8.00 %B 10.0 10.0 95.0 95.0 1 M ___________ ^00668 BEST COPY AVAILABLE Tuning Method Report Method: C:\MASSLYNX\SOUP020199.PRO\ACQUDB\PFOS3 Printed: Thu Nov 04 14:02:27 1999 Page 1 SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. Set Rdbk 1.60 40 5 0.2 150 250 1.62 -41 -7 150 250 Pressures Analyser Vacuum Gas Cell Rdbk 5.le-5 4.0e-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set 14.0 14.0 0.9 0.0 4 650 Set Rdbk 14.0 14.0 10 2.0 0.0 40 0 650 7 36 1 000669 cs \JOkMLTn\KXzroaoi9i .FROvacccDMUioM-rroa-poaA-prooA-x* L u t Modified: Prl Oet IS 10:39:03 1999 Printed: The sor 04 19:10:30 1999 doivent Delay ( alna ) ' 0.00 Ponction : 1 M M of 1 Maas Pair ( MSP* ) Inter Channel Delay i[ Seca ) : Span < Deltona ) : Start Tine { Nina ) : Bnd Tine ( Kina ) : Repeata : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Seca) Coll Energy (eV) Cone 1 413.00 109.00 0.30 30 IS Function : 3 M M of 1 Mana Pair ( MSP- ) Inter Channel Delay < Seca ) : Span ( Deltona ) : Start Tine ( Mina > : Ind Tine ( Kina ) : Repeata : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Seca) Coll Snergy (eV) Cone ( V 1 499.00 99.00 0.30 45 40 Function i 3 M M of 1 Maaa Pair ( M P - ) Inter Channel Delay i[ Seca ) : Span ( Deltona ) : Start Tina < Mina ) : Knd Tine ( Kina ) : Rapeata : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Seca) Coll Snergy (eV) Cone ( V 1 490.00 70.00 0.30 45 40 Function : 4 M M of 1 Maaa Pair ( MSP- ) Inter Channel Delay <( Seca ) : Span < Deltona ) : Start Tine ( Kina ) : Bnd Tine ( Kina ) : Repeata : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Seca) Coll Snergy (eV) Cone < V 1 427.00 00.00 0.30 40 40 Ptfft 1 0 0 0 6 *7 0 Mathod Report Nathod rilat Last Modified) Printed) Cl\KXaSLYNX\8OUJ020199.PRO\*CQUDBUOaln-10-95 Thursday, November 04, 1999 11)22)29 i Thursday, November 04, 1999 13i18i38 HP1100 LC Pump Initial Conditions Solvents A% B% C% D% 90.0 10.0 0.0 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 0.300 10.0 0 400 30.0 30.0 HP1100 LC Puna? gradient Timetable The gradient Timetable contains 5 entries which are : Time A% Bt C% D% 0.00 90.0 10.0 0.0 0.0 1.00 90.0 10.0 0.0 0.0 5.50 5.0 95.0 0.0 0.0 7.50 5.0 95.0 0.0 0.0 8.00 90.0 10.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 HP1100 LC Pump external Event Timetable The Timetable contains 3 entries which are : Time Initial 0.00 0.10 Column Switch Contactl Off Off Off On Off Off Contact2 Off On Off Contact3 Off Off Off Contact! Off On Off HP1100 JUitoaaavler Initial Conditions Draw Speed Eject Speed (ul/min) Draw Position (mm) Stop Time (mins) Injection Volume (pi) Vial Number 200.0 200 0.00 9.00 10.0 51 Page 1 Pressure 400 400 400 400 400 000671 Masalynx Sam ple List Sam ple List: C :\M A S S LY N X \soup020199.pro\Sam pleD B \110499a.SPL Printed: Thu Nov CM 13:18:22 1999 Page 1 P age Position: (1 ,1 ) File Name File Text MS File 1 110499001 MeOH Blank 1 0 M IN -P F O S -P O A A -P F O S A -IS 2 110499002 MeOH Blank 10M IN -P F O S -P O A A -P F O S A -IS 3 110499003 MeOH Blank 10M IN -P F O S -P O A A -P F O S A -IS 4 110499004 TO X145-R B S 11039-H 2O Blk-9, ext. 11/3/99 M CH 10M IN -P F O S -P O A A -P F O S A -IS 5 110499005 TO X145-R B S11039-Sera Blk-9, ext. 11/3/99 MCH 10M IN -P FO S -P O A A -P FO S A -IS 6 110499006 T O X 1 4 5 -R T S 1 1039-S era Blk-9, ext. 11 /3 /9 9 M C H 10M IN -P F O S -P O A A -P F O S A -IS 7 110499007 TO X14S-RBS11039-5ppb-9, ext. 11/3/99 MCH 10M IN -P FO S -P O A A -P FO S A -IS 8 110499008 TO X145-R B S 11039-1 Oppb-9, ext. 11/3/99 M CH 10M IN -P F O S -P O A A -P F O S A -IS 9 110499009 TO X145-R B S 11039-25ppb-9, ext. 11/3/99 M CH 10M IN -P F O S -P O A A -P F O S A -IS 10 110499010 TO X145-R B S11039-50ppb-9, ext. 11/3/99 M CH 10M IN -P F O S -P O A A -P F O S A -IS 11 110499011 T O X 1 4 5 -R B S 1 1039-100ppb-9, ext. 11/3/99 M C H 1 0 M IN -P F O S -P O A A -P F O S A -IS 12 110499012 T O X 1 4 5 -R B S 1 1039-250ppb-9, ext. 11/3/99 M C H 1 0 M IN -P F O S -P O A A -P F O S A -IS 13 110499013 T O X 1 45-R B S 11039-500ppb-9, ext. 11/3/99 M C H 10M IN-PFOS-POAA-PFOSA-IS 14 110499014 T O X 1 45-R B S 11039-750ppb-9, ext. 11/3/99 M C H 10M IN-PFOS-POAA-PFOSA-IS 15 110499015 TOX145-RBS11039-1000ppb-9, ext. 11/3/99 MCH 10M IN-PFOS-POAA-PFOSA-IS 16 110499016 MeOH Blank 1 0 M IN -P F O S -P O A A -P F O S A -IS 17 110499017 TO X145-R TS11039-250ppb-MS9, ext. 11/3/99 M CH 10M IN-PFOS-POAA-PFOSA-IS 18 110499018 TO X145-R TS11039-250ppb-M SD 10, ext. 11/3/99 M CH 10M IN-PFOS-POAA-PFOSA-IS 19 110499019 TO X145-R TS-9R 03240M -0-D ay 29, ext. 11/3/99 MCH 10M IN-PFOS-POAA-PFOSA-IS 20 110499020 TO X145-RTS-9R03241 M-O-Day 29, e x t 11/3/99 MCH 10M IN-PFOS-POAA-PFOSA-IS 21 110499021 T O X 1 45-R T S -9R 032 42M -0-D a y 29, ext. 11/3/99 M C H 10MI N-PFOS-POAA-PFO SA-IS 22 110499022 TO X145-R B S 11039-250ppb-CCV9, ext. 11/3/99 M CH 10M IN-PFOS-POAA-PFOSA-IS 23 110499023 MeOH Blank 10M IN-PFOS-POAA-PFOSA-IS 24 110499024 T O X 1 45-R T S -9R 032 43M -0-D a y 29, ext. 11/3/99 M C H 10M IN-PFOS-POAA-PFOSA-IS 25 110499025 T O X 1 45-R T S -9R 032 43M -0-D a y 29, ext. 11/3/99 M C H 10M IN -P F O S -P O A A -P F O S A -IS 26 110499026 TO X145-R TS-9R 03255M -5m g/kg-D ay29, ext. 11/3/99 MCH 10M IN -PFO S-PO A A -PFO SA -IS 27 110499027 TO X145-R TS-9R 03256M -5m g/kg-D ay29, ext. 11/3/99 MCH 10M IN -PFO S-PO A A -PFO SA -IS 28 110499028 TO X145-R TS-9R 03257M -5m g/kg-D ay29, ext. 11/3/99 MCH 10M IN -PFO S-PO A A -PFO SA -IS 29 110499029 TO X145-R B S11039-250ppb-C C V10, ext. 11/3/99 M CH 10M IN-PFOS-POAA-PFOSA-IS 30 110499030 MeOH Blank 10M IN -P FO S -P O A A -P FO S A -IS 31 110499031 T O X 145-R T S -9R 03258M -5m g/kg-D ay29, ext. 11/3/99 M C H 10M IN -P FO S -P O A A -P FO S A -IS 32 110499032 TO X145-RTS-9R03259M -5m g/kg-Day29, ext. 11/3/99 MCH 10M IN -PFO S-PO A A -PFO SA -IS 33 110499033 TO X145-RBS11039-250ppb-CCV9, ext. 11/3/99 MCH 10M IN-PFOS-POAA-PFOSA-IS 34 110499034 MeOH Blank 10M IN-PFOS-POAA-PFOSA-IS 35 110499035 TO X145-R B S 11039-H 2O Blk-9, ext. 11/3/99 M CH 10M I N -P FO S -P O A A -P FO S A -IS 36 110499036 TO X 145-R B S 110 39-S e ra Blk-9, ext. 11/3/99 M C H 10 M IN -P F O S -P O A A -P F O S A -IS 37 110499037 TO X145-R TS11039-Sera Blk-9, ext. 11/3/99 M CH 10M IN -P FO S -P O A A -P FO S A -IS 38 110499038 TO X145-R B S 11039-5ppb-9, ext. 11/3/99 MCH 10M IN -P FO S -P O A A -P FO S A -IS 39 110499039 TO X145-R B S 11039-1 Oppb-9, ext. 11/3/99 MCH 10M IN-PFOS-POAA-PFOSA-IS 40 110499040 TO X145-RBS11039-25ppb-9, ext. 11/3/99 MCH 10M IN-PFOS-POAA-PFOSA-IS 41 110499041 T 0 X 1 4 5 -R B S 1 1039-50ppb-9, e x t 11/3/99 M C H 10MI N-PFOS-POAA-PFO SA-IS 42 110499042 TO X145-R B S 11039-100ppb-9, ext. 11/3/99 MCH 10M IN-PFOS-POAA-PFOSA-IS 43 110499043 TO X145-RBS11039-250ppb-9, ext. 11/3/99 MCH 10M IN -P F O S -P O A A -P F O S A -IS 44 110499044 TO X145-RBS11039-500ppb-9, ext. 11/3/99 M CH 10M IN-PFO S-PO AA-PFO SA-IS 45 110499045 TO X145-RBS11039-750ppb-9, ext. 11/3/99 MCH 10M IN-PFO S-PO AA-PFO SA-IS 46 110499046 TO X145-RBS11039-1000ppb-9, ext. 11/3/99 MCH 10M IN-PFO S-PO AA-PFO SA-IS 000672 Massiynx - Sam ple List Sample Ust: C:\M ASSLYNX\soup020199.pro\Sam pleDB\110499a.SPL Printed: Thu Nov 04 13:18:22 1999 Inlet File Bottle Inject Volum e Sam ple Type Cone A C o n cB C o n c C 1 10m in-10-95 91 2 10m in-10-95 91 3 10m in-10-95 91 4 10min-10-95 1 5 10min-1O-95 2 8 10rnin-10-95 3 7 10min-10-95 4 8 10min-10-95 5 9 10min-10-95 6 10 10min-10-95 7 11 10min-1O-95 8 12 10min-10-95 9 13 10min-10-95 10 14 10min-1O-95 11 15 10min-10-95 12 16 10min-10-95 92 17 10min-10-95 13 18 10m in-10-95 14 19 10m in-10-95 15 20 10m in-10-95 16 21 10min-10-95 17 22 10min-10-95 25 23 10min-10-95 92 24 10min-10-95 18 25 10min-10-95 19 26 10min-10-95 20 2 7 10m in-10-95 21 28 10min-10-95 22 29 10min-10-95 26 30 10min-10-95 93 31 10m in-10-95 23 32 10min-10-95 24 33 10min-10-95 25 34 IOmin-IO-95 93 35 10min-10-95 1 36 10min-10-95 2 37 10min-10-95 3 38 10min-10-95 4 39 10min-10-95 5 40 10min-10-95 6 41 10m in-10-95 7 42 10m in-10-95 8 43 10m in-10-95 9 44 10min-10-95 10 45 10m in-10-95 11 46 10min-10-95 12 10 . 10 -- 10 -- 10 -- 10 -- 10 -- 10 - 10 -- 10 -- 10 -- 10 -- 10 --- 10 -- 10 -- 10 - 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 10 . 10 - 10 -- 10 -- 10 -- 10 - 10 . 10 -- 10 __ 10 - 10 -- . . ---- ---- ---- ---- ---- -- - -- . ---- -- . ---- . . ---- ---- . -- ---- . -- ---- ---- -- -- . ---- ---- ---- ---- ---- ---- ---- . -- ---- ---- --* . - . ---- -- . ---- -- __ -- __ -- . - __ -- __ . . -- . --, __ . . ---- . -- . . . . . -- -- -- . . . . . -- . -- -- -- -- -- -- -- . -- -- __ . __ __ . . -- __ _ __ . . . . . . . . -- Page 2 P age Position: (2 ,1 ) 000673 FACT: DATA REVIEW SUM M ARY FO RM Dale: Dala Analyst: FACT Study*: 7 5 */Vs- Matrix/Timepoints: Sam ple U se r- (ft* 2 1 A i t f r j j / t t . - <*</ ifasiiL_______________________________________ Set-up Analysis Dale/Analyst MMU 't/S-h Instrument % e. Analyte: PvfA C a f Acceptable Linear R a n Ha LOO. Ha Extraction Blank HA RA2: m Matrix Blank HA Calibration Checks: HA MS/MSD: _!l______________ Analyte: TPbS CCHz'* Acceptable Linear Ranne: LOO: *Kf-HOnn L 9%pL ft Extracted Blank /ss aa. Q RA2: 0. ?ffH Matrix Blank fas //**->Q Calibration Checks: OK ~ MS/MSD: Data Status: p< vW Gf.le .'O iL'lto Data Review Sign-Off Analyst Review Name / Date: Technical Review Name/ Date: A V S S t. / fyh N M ' l - f j Quality Assurance Review Name/Date:___________ Data E n try ; / \ \ , Costumata / Justifications: A cJikr*--lni fiur*e lots Y**- -ftr /< ttstL L _________ y re. <gtw4 u*-el te tjh * -_____ -( n a s a d v . -- J k i * / o ( / t f ______________________ -- Cii^ -jeisf-f^if a . / % 7 L LYr* fjtc fu r/ 40 "jU j MXre lAja. 4 L -i Zo*/ ccgy& cj ^ u j * a t A J - "Ju *dL>< jl JL ten-ts tere. enJuJ OlHr <L nuo-r tsuu l 4 L l L - * * * h f J /f 1 Z M , J / J J Ay- Ctm.n.f so-yin____A * * * L d** - -t*. J r i o * . ' J o < -^ik S "ArU*. Analyte: TfbSA (CH Acceptable Linear Range: -13 rtL LOQ: l& ffL Extracted Blank /(Ss Ja. * O Q R*2: - 9 9 1 7 0 8 Matrix Blank U ss -fLa.*, .& j Calibration Checks: OK z& _______________________ MSMSD: rilfr DttaSarus: L i i J i i ^ d . Tcntjinl'T 000674 FACT: DATA REVIEW SUMMARY FORM Dale: Data Analyst: Jas FACT Study t: fo i NS Mainx/Timepointx p j< * - r L 29 d u d & * l * i Sample List te S 1 9 Set-up Analysis Datc/Anaiyst HAU ' k i n Instrument y > 620! "k fa Data Review Sign-Off Analyst Review /, Name / Date: 3a* * / tm Technical Review p Name / Date: H ii\r tr t o Quality Assurance Review Name/Date:___________ Uc nM? Data Entry:. J L tJ rtf Ih jifl.ftf,___ U t llhlW Analvte: Su.rr Acceptable Linear Ranne: AJA LOO /J Extraction Blank: AM R"2: Ha Matrix Blank: N A Calibration Checks: MS/M5D: Data Status: MA --.____ - 000675 TOX14S-day2 control and dos*- matt. 11/3/99 Sanpla Lit : C :M4M8LXNX\sou030199 .pro\SanplaIM\110S99b U l t nodiCiod: Fri NOV 05 1S:2:11 199 Mntbod: c:\KBSit.a\aopoaoi9f .pro\MatbOBUl05ffb baa nodilad: Non Nov 0 07:09:59 1999 dob Coda: Printad: Non Nor 09 07:29:43 1999 rianimili l: F O U (Cbl) ana 1 110599029 2 110599029 3 110599030 4 110599031 5 110599032 6 110599033 7 110599034 9 110S99035 9 110599036 10 110599037 11 110599039 12 110599039 13 110599040 14 110599041 15 110599042 16 110599043 17 110599044 19 110599045 19 110599046 20 110599047 21 110599049 22 110599049 23 110599050 24 110599051 25 110599052 26 110599053 27 1105990S4 29 110599055 29 110599056 30 110599057 31 110599059 32 110599059 33 110599060 34 110599061 35 110599062 Banplaliat Tant MaOK Blank MaOH Blank MaOH Blank TOX145-RBS11039-H2O Blk-9, axt. 11/3/99 MCH TOX145-RBS11039-Sara Blk-9, axt. 11/3/99 MCH TOX145-RTS11039-Sara Blk-9, axt. 11/3/99 MCH TOX145-RBS11039-5ppb-9, axt. 11/3/99 MCH TOX145-RBS11039-10ppb-9, axt. 11/3/99 MCH TOX145-RBS11039-2Sppb-9, axt. 11/3/99 MCH TOX145-RB5U039-S0ppb>9, axt. 11/3/99 MCH TOX14S-RBS11039-100ppb-9, axt. 11/3/99 MCH TOX145-RBS11039-2S0ppb'9, axt. 11/3/99 MCH TOX145-RBSU039-500ppb-9. axt. 11/3/99 MCH TOX145-RBSU039-7S0ppb>9, axt. 11/3/99 MCH TOX145-RB611039-1000ppb-9, axt. 11/3/99 MCH MaOH Blank TOX145-RTS-9R03255M-5ag/kg-Oay29, 0:10 TOX145-RTS-9R03256M-Sag/kg-Day29, OtlO TOX145-RTS-K03257M-5MO/kff-Oay29, 0x10 TOX145-RTS-9K032StM'-5ne/kg-DBy29, 0x10 TOX145-RTS-9R032S9M-5nQ/k9-Oay29, 0:10 TOX145-RB$11039-250ppb-CCV9, axt. 11/3/99 MCH MaOK Blank TOX145-RBS11039-H2O Blk-9. axt. 11/3/99 MCH TOX145-RBS11039-Sara Blk-9, axt. 11/3/99 MCH TOX145-RTS11039-Sara Blk-9, axt. 11/3/99 MCH TOX14S-RBSU039-Sppb-9. axt. 11/3/99 MCH TOX14S-RBS11039-10ppb-9, axt. 11/3/99 MCH TOX145-RBS11039~25ppb-9, axt. 11/3/99 MCH TOX145-RBS11039-50ppb-9, axt. 11/3/99 MCH TOX145-RS511039-100ppb-9, axt. 11/3/99 MCH TOX14S-RBSUQ39-250ppb-9, axt. 11/3/99 MCH TOX145-RBS11039-S00ppb-9, axt. 11/3/99 MCH TOX14S-RSSUO39-750ppb-9, axt. 11/3/99 MCH TOX14S-RAS11039-1000ppb-9, axt. 11/3/99 MCH Standard Standard Standard Standard Standard Standard Standard Standard Standard QC Standard Standard Standard Standard Standard Standard Standard Standard Standard Std Cone 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 XT 7.172 7.174 7.192 7.177 7.153 7.172 7.147 7.117 7.155 7.174 7.131 7.106 7.172 7.151 7.152 7.170 7.195 7.173 7.175 7.192 7.196 7.133 7.198 7.133 7.172 7.147 7.141 7.171 7.146 7.152 7.153 7.174 7.131 i>. u<f A m a Plaga 28 bb 20 MM 17 bb 69 bb 54 bb 45 bb 48 bb 42 bb 39 MM 53 MM 61 MM 63 MM 57 MM 85 M4 87 bb 10 MM 16 bb 21 Mtf 32 MC 17 MC 45 bb 67 bb 61 MM 43 MM 41 bb 44 MM 45 Ml 38 bb 51 MM 58 MM 63 bb 77 MM 83 bb Cone. 0.49 0.35 0.29 1.20 0.93 0.78 0.84 0.74 0.67 0.92 1.06 1.09 1.00 1.48 1.51 -51 -65 -71 20 -7 -22 -16 -26 -33 -8 6 9 -0 48 51 0.18 0.27 0.36 0.56 0.29 0.78 82 -73 64 -44 -71 -22 1.17 1.05 0.75 0.71 0.76 0.78 0.67 0.89 1.00 1.10 1.34 1.44 17 5 -25 -29 -24 -22 -33 -11 0 10 34 44 oup 030199: Quantitated and printad by iaa on 11/09/99 000676 % j 5= i' T-'-TV H ? gSSSgSSSSSSSKS s s g s s s j r a g g g gs2S33SSPSS ^ ------s s M S K g - s ^ laaaaSSi2i2isSSsas |3 S S 3 3 3 3 3 S H g ||S |i 3 3 3 S 3 E g g MsssssssRss8sss533sa*SaS**asS sssssssss sssssssss ^000000^0 VV VV VV VV? TOOC145-doy29 control ad doso- w t . 11/3/99 S i^iiiiiip ""j 5|iiiiii;55*...SSSS5 SSSSSC? *5SP*!...SSSS? \% L I. * m OHO* MM* Isis f. BsSs ;i un r* s i $ aiwM wM |ljli ? lilis i s = --s s i i m ..Vjill IM ii* lili m i S i " n i 1.-.-.-., 2L -n n m iiitii 1liliiliiliilililiiiiiiiiiii *! s s s s s s s s s s l s SS3q333535SSaSSSSRS5SaaSSS 000677 000678 SKSSSSSSSKSSSSaSUECCCg ":m h h m p ;; =s==esgsg!;c Sssss' %;;iE EEE ;s s s S S S - $ ^ gs!s??s<s??s!s? " 5EEEssss S55 |S55!5 m TM % \ ftpitprtrtt "SS3SS.. ggggsssis Ek s s s s e - . gggggssb ===5=S=5SS=S=====S=5===5S=5=25SSs llllIlilaSSSsIsgSSlIIlIissISSsis BBBEBBBBBBBfl&BBBBBBBBBBBBBBBBgB&m| 3ssscBgs.....s...-- sb-SSss-.-o..b.| SSSSSSSEggggSgggggSSgEKSSSSggggSS? OOHUfciMa i ,,,,oi f *9 ^ V \ %\ i i I It & 9 { 8 ^9000 SSKPSSSSSStiSSSSSKGCCGtS. Ilslssll iiiiiliii mmmmmm Illlls ls s s lllls l CSSSSSSKSKS ! i 1 g s s s s . ^..5 " S s s s SS5 ' " i h h ; PHHHMHHHH ggggggggg m g SsESEESEESss HESsSsSSsEissssEEsE S3 I eI eI I eeI I gs&mg&sm E E s E E g ^ lH l mmsmmmsKS S *1 OOHHHOHHSOHO MOOOOOOOOMHMOHMOOOO ssggbsssssss sbbccbsissbsgssgsgss ,,..s 00 s? sf ? _______________________________________________________ :________________________________________ 3 * * /sin j . U / Quantify Calibration Hapert TOX14S-day29 control and doaa> out. 11/3/99 1 ooogso Quantity calibration import T0X145~0*y29 ooatrol and dona- ant. 11/3/99 3 000681 Quantify calibrano import 9Q0tl4S-day29 control and dosa- ant. 11/3/99 papo 3 0006^ Quantify Calibration Kapert TOQU45-ay29 control and dosa* axt. 11/3/99 J Me* * 000683 Method Rpare Method f -a : Last m od ted: Compound. Printed: 2C :\M7. iL Y N X V s o u p C 10199.pro\MethOB\110S99b.mdb Mon in C 37:C9:5S 1999 1: A A ;Cal) K c a : ; / 03 17:2?:>4 1999 Compound Name: Internal ?.: Quantify Trac: Cone, of Standards: a*r RF valu: User Peak Factor: Integrate Window Factor: Chromatogram mass windev: pcaa :c>ii) Fixed l.OOCOOO, Disabled 1.00C30 2.053 i.o::3Da Retentior rim* (mins Relativ* rtention 7 RT Refer- :: Tim Wir .a (mins): Peak Selection: enabled Disabled iv.z.\ Response Type: Response: external Area, Polynomial Type: Point of Origin: Pit Weighting: Axis Transformation: Linear Exclude 1/X Ncr.e Units: Peak-te-r-K aag>litude: 1Cj Smooth ir-. Window si.e (scans): Number c: smooth*: Smctthir. rethod: r.-.sl.led 1 Join vail threshtld: Reduce pc~k tailing: Raise basilir.* maximum: 1C .1? Drew vert teal threshold Detect sr tulders: Shoulder threshold: 90.c: Disabled 30.o: Relative ' . - i g h t : Absolute sight; Relative 3rea: A b s o l u t - tea : 1 . 5 3 . Disabled zi ..;:od.. Disabled Disabled :.?:. Disabled /> M f 1' Rag* BEST COPY AVAILABLE OOO684 Method lu.-ort Method file: Last modified: Compound: Printed: C:\HA SSl-YNX'.soupC20l99.pro\MethDB\110S99b.mdb Mon ?:'v OB 07:15:33 1999 2: P.-'is ich:: Mon :::v 03 17:25:>4 1999 Compound :N a i m s Internal Ref.: Quantify Trace: Cone, of Standard: User RF Value: User Fea>. factor: Integrate window Factor. Chromatog-An mass window PFCS Ch2) (None! t :c Cone. A 1.001700, Disabled i.oc: .00 i.c::13a Retention Time (minr' : Relative mention virr* RT Refer* .Cc: Tima Window (mins): Pea'c Selection: 7.:::. enabled . Disabled ; 3.522 ::car?3t Response Type: Response: Polynomial Type: Point of Origin: Fit Weighting; Axis Tra; jicrmatior.: linear Sxclui* 1/:: ::ene OnitS: Pealc-to-T - amplitude: Smoothing: Window sire (scans}: Humber of smooths: Smoothing method: Scat led 1 Join valley threshold: Reduce p<*< tailing: Raise ba^-sli..d maximum: 21?.10 s.:i Draw ver-Lc'. threshold: Detect s .drs: Shoulder .'.reshold: Disabled 33.c: Relative -:jht: Absolute sight: Relative .a: Absolute rsa: L.:l. Disabled 1.11. Disabled 2.00. Disabled Disabled Page 2 1 BEST COPY AVAILABLE 00068S Mathod Report Method fileLast modified: Compound: Printed: C:\MA3SLYNX\s=up0:0199.pro\MethDB\110599b.*db Mon Kcv 08 07:03:33 1999 3: PT3SA (Ch31 Mon hav 08 07:23:34 1999 Compound Name: Internal ?.ei.: Quantify Trace: Cone, of Standards: Osar RP Value: User Peak Factor: Integrate Window Factor: Chromatogram mass window; PFDTA <Ch3) [None 1 TIC Cone. B 1.000000. Disabled t.OGOOOO 2.000 l.OCUDa Retention Time (mini): Relative Retention Tire: RT Reference: Time wir.iow (mins): Peak Selection: 1.1`z. enabled ..;.D, Disabled idcr.e) :.i6S Nearest Response Type: Response: External Are.*.i Polynomial Tyne: Point of Origin: Pit weighting; Axis Trarricrration: linear Exclude 1/3C done Units: Peak-to~r*< amplitude: Snoochin?: Window sire (scans): Number of smooths: Smoothing net nod: Enabled 2 1 Join valley threshold: Reduce pe >v. tailing: Raise b a s - 1 m a x i m u m : Draw vert.?1 threshold: Detect sh .'.cers: Shoulder rhold. 90.00 Disabled 30.00 Relative height: Absolute r.eigiit: Relative area: 1 .3 0 . Disabled , Disabled 1 .0 0 , Disabled Page 3 * BEST c o p y a v a il a b l e 000686 Method Report Method f i l e : Last m odified: Compound: P rinted: C:\MASSLYNX\so-.; -'2 0 19 9 .p ro \ M a th D S \ 110 5 9 9 b .m d b Mon Nov 09 0 7 : I > .58 1999 4: S u rr (Chi; Mon Nov 08 0 7 ;2 ? :5 4 1999 Compound Name: I n te r n a l ?..: Q u en tiiy Trace: Cone, o f Standards: U se r RF V a lu e : User Peak F acto r: I n t e g r a t e Window F a c to r : Chromatogram mass window: S u rr (Ch4) i::sr.e} F ix e d 1 . C77000, D isab led 1 . ciiio o 2. c :: l.G .lO D a R e te n tio n Time (m in s): R e l a t i v e i n t e n t i o n Time RT R e fe r e n c e : Time Window ( m in s ) : Peak S e le c tio n : Enabled 1 . . . . D isabled 0 .2 * 7 N earest Response Type: Response: E xternal Polynom ial Type: P oint o f O rigin : P i t Weigh---.nr: A xis Transform ation: L in ea r E x clu d e l/>: iicr.e U nits: P eak-to-peak am plitude: Sm oothing: Window s i z e ( s e a n s ) : Humber o f sm ooths: Smoothing r-ithod: E na-led 1 Join v a llt y th resh old: Reduce pe t a ilin g : R a is e b a s - t '.ir e maximum: i .; .: d Draw v e r t i c a l t h r e s h o ld : D etect sr.: .Id e rs: Shoulder th resh o ld : R elative h eigh t: Absolute e ig h t: R ela tive area: Absolute area: 9 3. 11 C. 2. Cl 0. 21 " O isobled D isabled D isabled D isabled Pag 4 BEST COPY AVAILABLE 000687 Quattro II, #6414E SOUP 020199: FACT Equipment Log 99092 PAGE 1/1 DATE: 11-05-99 ANALYST :mmh STUDY NUMBER: TOX145 MATRIX: rat sera DESCRIPTION: day 29- dil FACT Method: ETS-8-5.1 Injection volume: 10 uL Cycle time: 10 min. Electrode: Z-Sprav Mobile Phase: (A12.0 mM NH4CH3CQ2 (B) MsQH TN-A- or stndrd number (A) 99085-11-15_______ (B)m -A-?22I Prepared (date/by): (A) 10/30/99 sah_______ (B )juom sah- Expires: (A) 04/00______________ (B) 2010______ Store at room temp? @ or N Other:. G uard column: None__________________ Part number: na_________ Lot number: na Analytical column: Keystone Betasil___________________________________ Size: 2 x 50 mm________________ Type: C18___________ Sphere size: 5 um Part number: 055-701-2_________ Lot number: P9E1I Serial number:0591804Z Analytical parameters: Drying gas (L/hrl: 350 ESI nebulizing gas (L/hrl 13 LC Flow rate: 300uL/min. Backpressure: 65 bar Sheath gas (L/hr)_Q. HPLC solvent gradient: lOmin-10-95 Tim; (min,')____ DJLQQ__________ 2H .0 0 3)_L3Q________ 4 ) JLSQ__________ 5ILQQ_____ %B JM 1M _ _22iL 2LL ma. 0006S8 BEST COPY AVAILABLE Tuning Method Report Method: C:\MASSLYNX\SOUP020199.PRO\ACQUDB\P7OS3 Printed: Pri Mov 05 15:32:05 1999 Page 1 MS SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. MS2 Set Rdbk 1.60 40 5 0.2 150 250 1.60 -60 -6 149 249 Pressures Analyser Vacuum Gas Cell Rdbk 5.le-5 4.le-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set Rdbk 14.0 14.0 0.9 0.0 4 650 3 Set Rdbk 14.0 14.0 10 2.0 0.0 40 0 650 42 40 45 000689 c anning Method Report Method: Ci\iauisLyia:\goaoaoitf .vRoucoaosMoicza-rroc-MJkA-rTogA-za * LCCfe Modified: rri O ct. 15 10:35x03 1999 Printed: rri Bov 05 15:51x35 1599 Mirant Onlay ( a i u ) : 0.00 0% 1- ! Function x 1 NRM Fair ( Bar- ) Inter Channel Delay 1; Secs > : Span ( Daltons ) : Start Tin ( Kins ) : Bnd Tine ( Kins > 1 Repeats : Channel Parent Daughter 0.01 0.00 0.00 10.00 1 Dwell (Secs) Coll Energy (eV) Cone 1 411.00 169.00 0.10 30 IS Function : 2 MKM of 1 Mas* Fair ( BSP- ) Inter Channel Delay ( Secs ) : Span ( Daltons ) : Start Tine { Mins ) Bnd Tine ( Kins ) : Repeats : Channel Parent Daughter 0.01 0.00 0.00 10.00 1 Dwell (Secs) Coll Baargy (eV) Cone 1 499.00 99.00 0.10 45 60 Function : 5 aaiM of 1 Mass Fair ( BSP- ) Inter Channel Delay 1( Secs ) : Span ( Daltons ) : Start Tina ( Mins ) m ad Tine ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 IQ. 00 1 Dwell (Secs) Coll Energy (eV) Cone 1 495.00 75.00 0.10 45 60 Function x 4 m o m of l M u * air { Bar- ) inter Channel Onlay ( Seen ) s Span ( Dalton* ) ; Start Tine ( Mins ) : Bad Time ( Kins } : Repeats : Channel Parent Daughter 0.01 0 .0 0 0.00 10.00 1 Etoell (Secs) Coll Energy (eV) 1 427.00 50.00 0.10 40 Cone ( V ) 50 fm gm 1 000690 Masslynx - Sample List Sample Ust: C:\MASSLYNX\soup020199.pro\SampleDB\110599b.SPL Printed: Fri Nov 05 15:26:20 1999 Page 1 P ag e Position: (1 ,1 ) File Name File Text MS File Inlet File 1 110599028 M eO H Blank 10M IN-PFO S-PO AA-PFO SA-IS 10mln-10-95 2 110599029 M eO H Blank 10M IN-PFO S-PO AA-PFO SA-IS 10mln-10-95 3 110599030 M eO H Blank 10M IN-PFO S-PO AA-PFO SA-IS 10mln-10-95 4 110599031 TO X145-R B S11039-H 2O Blk-9, ext. 11/3/99 M CH 10M IN-PFO S-PO AA-PFO SA-IS 10mln-10-95 5 110599032 T O X 145-R B S 11039-S era Blk-9, ext. 11/3/99 M C H 10M IN -P F O S -P O A A -P F O S A -IS 10m in-10-95 6 110599033 TO X145-R TS11039-Sera Blk-9, ext. 11/3/99 M CH 10M IN-PFO S-PO AA-PFO SA-IS 10min-10-95 7 110599034 TO X145-R B S 11039-5ppb-9, ext. 11/3/99 M C H 10M IN-PFO S-PO AA-PFO SA-IS 10min-10-95 8 110599035 TO X145-R B S 11039-10ppb-9, ext. 11/3/99 M C H 10M IN -P F O S -P O A A -P F O S A -IS 10m in-10-95 9 110599036 TO X145-R B S 11039-25ppb-9, ext. 11/3/99 M CH 10M IN -P F O S -P O A A -P F O S A -IS 10m ln-10-95 10 110599037 TO X145-RBS11039-50ppb-9, ext. 11/3/99 M CH 10M IN-PFO S-PO AA-PFO SA-IS 10mln-10-95 11 110599038 T O X 1 45-R B S 11039-1 OOppb-9, ext. 11/3/99 M C H 10M IN -PFO S-PO A A -PFO SA -IS 10m ln-10-95 12 110599039 TOX145-RBS11039-250ppb-9, ext. 11/3/99 M CH 10M IN -P F O S -P O A A -P F O S A -IS 10m in-10-95 13 110599040 TO X145-R B S11039-500ppb-9, ext. 11/3/99 M CH 10M IN-PFO S-PO AA-PFO SA-IS 10mln-10-95 14 110599041 TOX145-RBS11039-750ppb-9, ext. 11/3/99 M CH 10M IN-PFO S-PO AA-PFO SA-IS 10mln-10-95 15 110599042 TO X145-R B S 11039-1000ppb-9, ext. 11/3/99 MCH 10M IN-PFO S-PO AA-PFO SA-IS 10mln-10-95 16 110599043 MeOH Blank 10M IN -P F O S -P O A A -P F O S A -IS 10m in-10-95 17 110599044 TOX145-RTS-9R03255M-5mg/kg-Day29, D:10 10M IN-PFO S-PO AA-PFO SA-IS 10min-10-95 18 110599045 T O X 145-R TS -9R 03256M -5m g/kg-D ay29, D:10 10M IN-PFO S-PO AA-PFO SA-IS 10min-10-95 19 110599046 T O X 145-R TS -9R 03257M -5m g/kg-D ay29, D:10 10M IN-PFO S-PO AA-PFO SA-IS 10min-10-95 20 110599047 TOX145-RTS-9R03258M-5mg/kg-Day29, D:10 10M IN-PFO S-PO AA-PFO SA-IS 10min-10-95 21 110599048 TO X 145-R T S -9R 03259M -5m g/kg-D ay29, D:10 10M IN -P F O S -P O A A -P F O S A -IS 10m in-10-95 22 110599049 T O X 1 45-R B S 11039-250ppb-CC V9, ext. 11/3/99 M C H 10M IN -P F O S -P O A A -P F O S A -IS 10m in-10-95 23 110599050 M eO H Blank 10M IN -PFO S-PO A A -PFO SA -IS 10min-10-95 24 110599051 TO X145-R B S 11039-H 2 0 Blk-9, ext. 11/3/99 MCH 10M IN-PFOS-POAA-PFO SA-IS 10min-10-95 25 110599052 TO X145-R B S11039-Sera Blk-9, ext. 11/3/99 M CH 10M IN-PFO S-PO AA-PFO SA-IS 10mln-10-95 26 110599053 T O X 1 45-R T S 1 103 9-S era Blk-9, ext. 11/3/99 M C H 27 110599054 TO X145-RBS11039-5ppt>9, ext. 11/3/99 M CH 10M IN-PFO S-PO AA-PFO SA-IS 10mln-10-95 10M IN -P F O S -P O A A -P F O S A -IS 10m ln-10-95 28 110599055 T O X 1 45-R B S 11039-1 Oppb-9, ext. 11/3/99 M C H 10M IN -PFO S-PO A A -PFO SA -IS 10mln-10-95 29 110599056 TO X145-R B S 11039-25ppb-9, ext. 11/3/99 M C H 10M IN -PFO S-PO A A -PFO SA -IS 10min-10-95 30 110599057 TO X145-R B S 11039-50ppb-9, ext. 11/3/99 M C H 10M IN-PFO S-PO AA-PFO SA-IS 10mln-10-95 31 110599058 T O X 1 45-R B S 11039-100ppb-9, ext. 11/3/99 M C H 10M IN-PFOS-POAA-PFO SA-IS 10mln-10-95 32 110599059 TO X145-R B S 11039-250ppb-9, ext. 11/3/99 MCH 10M IN-PFO S-PO AA-PFO SA-IS 10min-10-95 33 110599060 TO X145-RBS11039-500ppb-9, ext. 11/3/99 MCH 10M IN -P F O S -P O A A -P F O S A -IS 10m in-10-95 34 110599061 TO X145-R B S 11039-750ppb-9, ext. 11/3/99 M C H 10M IN -P F O S -P O A A -P F O S A -IS 10m in-10-95 35 110599062 T O X 14 5 -R B S 11039-1000ppb-9, ext. 11/3/99 M C H 10M IN -P F O S -P O A A -P F O S A -IS 10m in-10-95 000691 FACT: DATA REVIEW SUMMARY FORM ^r/tt/rt naie Dala Analyst: FACT Study It: Matrix/Timepoints: Sample List: Set-up Analysis Date/Analyst: 1* 4 . E J - L * s s ra< J r J s* } e*. "it*/ f f M f f f tk------------------------------------- Data Review Sign-OfT Analyst Review Name / Date: . <V /r/W Technical NameIS T T m r i f , , / Quality Assurance Review Name / Date:___________ Data Entry:. U c iphilw 000692 FACT: DATA REVIEW SUM M ARY FORM fi u h ^ .2 .n H a le Muffi Dala Analyst: fits FACT Study#: 7 Matnx/Timepoints: <{f f i t J L o i s , Sample Lut: /QK9a- i/jA t f t Set-up Analysis Date/Analyst: Instrument b fffff9 3i 2L 5) Analvte: 3 s ( c H i f Acceptable Linear Range: M A LOO: MA RA2: M A Calibration Checks: MA MS/MSD: Data Status: ~~ Extraction Blank M l Matrix Blank M A Analvte: Acceptable Linear Ranne: LOO: RA2: Calibration Checks: MS/MSD: Data Status: Analyte: / / Extracted Blank / Matrix Blank / / J s r f l g j <c, / / z Extracted Blank:. Matrix Blank: Data Review Sign-OfT Analyst Review Name / Date: 34-S H i t f a Technical Review Name / D ate:_____ A W -- Quality Assurance Review Name / Date:____________ ___ L e L ------ 10jul <1- Data E ntry:. I k L ___ I n i a i h l Comments ! Justifications: ,L-fns - Qtu. d- 4 ft Cq*fy* S ty L m s LaL & *-**& **} A SMutMytaJc 'ffaA */usJ*s4 faA (JL TftSA y to js m a s k J -tc c r f A v Q yks-____/h //*Ks/i-Jy Afa }*oJeL f a s h J dtSC oU evtJ. " J * $ t f / t h f (3 Area. &>n.nJ% />>- ~fh. TSri> - j j ----------------------------------------------U X iftr >% & c c e * -f 'ffa & 0 i f a J s aJ ucI V ii < 4 f j% . - - * e V / r / ? / f S td ir J O f c L tc k b j 6- k f a U c Ma s u x s J /k A f a S tM A jf VU.*. / - A n jflC .1 h jla * . o f fo -v/jA iM V - CS) f*0AA A P 4 M /g fJ q . APF ,/a , jy &n,___ o / r ______________________________________ ^ ( "eA-r.^C AVAIL'S- Alfr /o//g/9y L ^ a .-v \x X AfAk- / / J / f e s 4 A^sxSAA^ 10 AJQ-TA -vne*-r Ash iW = s Ajtrr -rS Ai* 000693 Soup 0201**: Quantified mad printed toy S S g S S X S S i S S S S S S S E E S E E E K i i S S S ESEEESESSSSESEEKES.,-,.,.,...^.-. % r m i p m * i f s H |? ? ? ? ? 11???? . , 5*** I P im p F p H P P p f_ "S**883" I !!" i Si! ;(H SU SU """li p 8 "bbbb 8 Sggggg S : g flll SSSSSS ssg55 1o3 SEES E SSE S S?M?r* * * * * * SEES ESEEE E"***'** ssS SpSS 5333 33333 3 3333 | | | | S - tBa to toI nMrt to trti rWt to ?Qi nQ nQ nQ Qo n O 5 r* Isisiss E S S S S SSSSSSSSS S 3 SS SS SS isS S S S E S ui SSSSSS33S -0 vt> ! lili S siisi! glissi S3ES53 EliiSslislilssli B SSESSESES s ESEES E SSSSSS s SSKK 5EESS S-SESSSEESKSKESEES 5 S 5 5 5 ? 3 S55&S 5 3 33 5 3 3 ? g i m s 5SS3S5 g 3 3 g g 5 5 g 3 S 3 3 3 3 3 g g 3 r sssssslso s oSS =S o & m s s l l i s SoJsS SoEosIoSoSSSSSEooS SS3SES3SS 3 SSSSE s K5KSK 3 3SS53 SSSESS SSSSS3SESSSC3ES3SS ooo 'vEsisli i i CP SS 8 skesSees 05 C> I t l 8 R l i* c O Oo <T ) cn t<3> r-* Si. o- tr 6 br r v\ ? ir c- o * ~o 'v ir iiuui4u<uuu< oooooooooooo WUIIDAAUIWUMAUIUIUI w OOOOOOOOOOOO hwMpoa4uw ` 0X>U)vllM^UKIH04(S-JmUli oooooooc l O O O O O O O O O O O O O O O O t 300000000000B _S O_ O_ O_ O_ O O O O O O O O O O O KUMfl U ___ OOOOOO IuH<i UietiUIaIA<U<Ic0Ui OOOOO IoU<i IedWMtIAoOMIU'OIdWi4eM `McU>WIsiWUfli OOOOOOOQO l ..............................................>...U...M....H.....0...4.....C...g.-HJOHIU 33333333383$ bbbbbbbbsbs 3K8K3X3K 3X S3$333333$3S333333$333388$333333$33333333333SS$8 5BSBBBsisEBSSBBBBBBBBgEBBBBBBBBSBBSBssBii tMItMMMMIVHBIIB IK U< 0 Ul UMl Vi RUlUIWUtUUIVu I95I 3 B 3 3 3 B B B S 5 SS 3 S S 9 7 M Sw&wfcw&w&xw* rrprrpprr r * r' J r' JrH rH f #r *- rW Hr rH Hr Hr r-I ooooooooo ww ww w w wM itf OWOUIOOU*C~ mo o e o o v ---- gHP H H H* * m MN H M !SS8" o (- w uoodo w w uu I MNNN N MVIIMKW sss^e E siili oo+ x w # t r M` 1 N B U nU "8888 'OOOOC oacxxxx fsssss imi III M N M M W W t) "88888 * H - H o o oo MO OH oH Ho Ho H - H* t w w ww HHHHH WW WWU <W59BRBXX;oSaMS 'r p d 53 02 02 02 K 3 ! 3 ! i i ! * ' 2r*!t*l dr lp! dt*:r * ' r rb ir i ri tpt iri Vp BpVrBr Br i n r S r n <>ldV'W . ^ J MNM ^ UMi <U OOOOOOOOOC wsSxxU O W U I Q O 3O O O C BW UUUW i UU U MN p-JiKMHwNHMr; S S S S S S S S S S S S 6 S S E S Oe IoKoD eI Ue CaOU o q <i>oH og ggcr* 7 5 nnnn grgggs pi o o o o M J H H1 *v I < F~m s s s 7 5 5 5 5 5 Qh h h p h flftoon' fnnnno S saato o o r e o o o o o i nnitr' mB B B BO t Bftrtftn mllrzis:? m -*- p**-** - - mM rPr -* M5 I * ( AWWHKP CAWMWHNHH P MHMMMH N M *- > MMm MH *-> *-* *r w * j w i lag* * * h t * 0004 * M H H H *1 * 0 0 OOO BS MH H H M MI I I l T 8 fem <o 8 .... 8 8 8 8 8 "SHbbs 8 8 SVifiS H M P H Ho Po Ho Ho Ho t- *4 - K B fi e 88 88 88 [fili Ili U4IIW K M M H O M BiW h I <40U>JWh 0 3" -V >o jO>jNls|gs|s]s MWn gMWwMMHWVtMgMOUWWMUW4' V*M'HMJ gMMB*k Jk4Mk)MUo IW^I>MHUMUo MIgBMg<AMHWMwgWMMUeMIK<i JWMMMMMMMMUUMMMMMWMMMMMk UBBgOBOHgpkUBOBHWOMNUIMt I MNMWMMb NNH W<bg> 0i MH HBM WB M *4H *J M*-* UIHABUMP HHgMW 0> f l P M U B U *4 fl H A 4 4 *4 H * J P4 PBPBBBMH g H W W N A a o g g A 4 P W A g g A H A O W U O l M U IB 4 B W A a U I4 > B B W B W W 4 V IB H W O W U I 4 V lV U U iy4 A fcH M IA U *> O H B tlM U O M W W W 0 A U M W 4 4 W W W H O W a g A A H a 4 4 V IA 4 U lfca B W W U IW 4 sai g m ig ig g ig m m s m m m E im m im ? K im m P ? g ffiS g l!g g S S im I MMMM MHMM H U H 9> *4 * o a u iu * *4 H OBBWP M W B 4 A W 4 M 4* Ot H* M M U M M M M M hi H4 AWH OMMS MWW k b V I M H P U> h N 4 B P O U* h h H WA 4 M h i hi Ol WHOKBMflU Q ONOUUpMOAB4l>APMOhOMtJ|lAHOBO4l)lAUUIOBeHBOOBBe0OOO*UBhOBAANOOOOOO[ lOWO o I- ,*Unn^ & t ;i <5>l *rr r s i F a- o % Q_ r S cn <j> s ~t f ol L 969000 66/9I/0X *T M P03*T* Po POTJI3o0 :66X050 *t *M>fa ^ 7f0 t '/o , ' T f f 00 1 ' ^ f> 6 /tf/o i ' OVl 9 H 'tn 7tf TfO ^ ip m y a CX- S 0 C 9 0 T 8X- 81*951 T 91*919 c - 10 00C P- S69XT t - 1 9 '0 9 PZ C t ` 9 t PX- P9 ` 01 X- 0*5 00*0 8Z- 66 *6 IZ e ro o c - 6Z *PTC 11r 6 6 * OOPZ * s o z K l i 9P *P1ZZ V SC166T 00*0 6 1 - 61*9XZ I l *0 LZ- 9Z C Z Z j.9 X Z Z 7 6CPS8P w fcTcvi\l1vIoiSre'ptPzztctePst 00*0 95- Z6CCZ 00*0 61- P Z lP Z rt(V-. 9 1 *PSPP ZZ'LIZ erzez zi* x tz ZO'ZXC 00*0 1 5 - 9 *CPZ .00*0 , 59 ' P (~ *z9 * o pc z 00*0 s tz OO'O XZ- 1 9 ` XtZ OO' O 00*0 OO'O OO'O OO'O OO'O *c x - S9 ZtOT ZX- '9 0 9 0 0CST9 0 91*90t T- 61*ZZI 9- P96S pz e r o e iz - '6 OP- Oi*C OO'O OO'O OO'O S Z 'P OO'O A*a% * 9000 XMt 69CSC noi ttz sz NN 6S90Z UN TCTOT 101 9CX9 IDI SO Zt MI 9PX MK XfiS ZXK 9C NK 9PX NK 09P 1 NK XTZ WC Z6Z1 qq 6 9 9 6 L PP 99Z99 PP 96PC1 q q 0XC99 NK CL1 WC tP P NK ZOZ NN 69S 1 >M ZC6 qp $6091 qq 6069SX P P ClZCST PP tlP9X NK e t x NN X96 NN e s t NN Z i t i qp bp9ipt NN 69C MH I t t i NN PZS6 KM 9Z50X NN CZT NN 1C9 NN C9X NN z s c qp T9 MI PT POI I L I NK SOI m i to te MI ZI NN OPt NK Z I MI CTI MK PT MI 991 n o i coisc n o i Z069Z NK 59S0Z NK 96C0X NK C9ZP MI t i l t MI 69H MI ZZ noi ire MI SI MI SPI POI BIT qq set pq x MU MT C *0*4 0X9*1 ZX9 ' Z61*l tT 9*l CX9 *L 6*L*L 0 6 ` X6 ' 9C 91 68 ' 0990 X 9 * 1 *i P091 0 6 ' ZX9*1 909 ' 9X9 ' 619*1 0X9*1 199*1 Z 6 1 '1 59*1 PX9 *1 tir i 909 1 909*1 1S9 *1 o ri es9*i tlB 'l 09*1 1X9*1 PX9 'L CIBI C iri ssr i 609*1 c e ri 1S9 *L 091 tC B 'l PZ9* 1 P1B*1 tX B 'l CX9*1 CX9` 1 se ri tt e 'i ZS9 ` 1 999`1 9 0 9 '1 CX9 '1 091 9X9*1 909*1 Z C l'l S09 *1 c e ri 991*1 09*1 961*1 6CB*1 958*1 0X9*1 ai 009ZZI 00*XZ6 00*9X9 0 0 'OC 0 0 * PCX 00* Z9 OO'XC OP'ZX PX *9 O O 'lO t 00*10C OO'lOC 00* o c OO'lOC OO'lOC OO'lOC OO'lOC oo*9zn 00*156 00*9X9 OO'lOC 00*951 00*59 OO'XC OP'ZX PX' 9 0009 P39 pxopooqg pjvpv*3t pxopcrog P3VpV>39 P*Op0039 P30p038 pjtopuosg pjopuoqs pxopaoqe 30 30 30 30 30 30 30 30 pxopaoag pxopooag pjcvpw 39 pxopuoag pxopuoag pxopooas p jo p u o ig p30pU03S p30pC03g d lt n s *xi-qtfoooT -cioT n99 ' spixox B IS , ll- q < M 0 S l- 6 C 1 0 t'1 9 'StXXOX BBS 'T I - q t M 0 0 S - 4 C I 0 n 9 'SPXXOX BBS 'TX -q4dO SZ -6nO T *19B 'SPXXOX n s 'T X -q00X -6C 10T *W ' spix o x BBS ' l!-q a 4 0 S ~ 6 C I0 I * lflB -S P IX 01 n s 'n - q M s z - 6 c i o n a B 'sp x x ca, ix e 'x x -q q ^ o T -s c io n e B ' spixo x BBS * T X - q d S - 6 C 1 0 n a s 'SPIXOX HUI8 HOH n s * 9 -T I-A 3 O -q * * 0 S Z -6 e T 0 T lB 'SPXXOO. 3U 18 HOH n s 'P -X T -A 33-q< M 0S Z -6C 10nB a 'SPIXOX 66/C X /0X n s - S q / t e s '9 * 3 ,N9SZtOB6'*IO.B 'SPIXOX 66/C X /0X n s - o q / f t n 5 'P ^ a 'N tSZtO B6-*lX B SPIXOX 66 /C X /0 X n s - S q / t e s 'P ^ a 'KZSZC0B6-*IXB 'SPIXOX 6 6 / t l / O I n s - A q / t e s `r*a 'K ISZC 0B 6-*U B 'SPIXOX qu*TS HO*N n s 'P -T T -A 33-q< M 0S Z -6C T 0n9B 'SPIXOX q ttv iB HO*H U S 'P - I I - / O 0 - q 0 S Z - 6 t T 0 n S B 'SPIXOX 6 6 /rx /o x n s -A q/es `p*a 'H o s z c o s s -ix a ' spixo x 6 6 /C I/0 X n s -B q /B v s lA a 'N6PZC0B6-1XB 'SPIXOX 66/CX/OX n s -Aq/Aapj `1*3 *N9PZC0i6-lXa 'SPIXOX 66/C T /O X n s -A q/O iiS 'l A a *HlPZC0B6-nXB SPIXOX 66/CX /O X n s - 6 q / e s lA a *M 99ZeOX6'*U SPIXOX q u t a HOH n s 'C -IT -A 3 3 -q < M O S C -6 n o n 8 * 'SPIXOX q u i a HO*H n s *C -IX -A 3 3 -q q q o S Z -6 C I0 n B M 'SPIXOX 6 6 / c x /o t n s -A q/ow s * t* a 'N s p c c o n e -ix a spix o x ZX -O SM -qd06C-ie33D O O 'Aq 'HSC5C0X6 SPIXOX B t-S N "q d 0 S Z -IO 3 3 a o D 'A q 'KSCZC0B6 SPIXOX X X -O S M -qdO fiZ -Ioxaaoo ` xAa 'K0CZC0B6 'SPIXOX XX" S K -q q 0 S Z -IO O O 0 'l A a 'K0C5C0B6 `SPIXOX q ir x s HOW BBS 'Z - I X - A 3 3 - q < M o S Z - 6 tI 0 n 8 B SPXXOX 66/CX /O X n s > x o a a u o o ' p / a 'K6CZC0B6-1XH SPIXOX 66/CX /O X n s -IO 33U O 0 'p A a 'H9CZC0B6-1XB SPIXOX ns66/CX /O X - x o m z e o 'piCa 'MICZCOBS-'U * s p ix o x 66/CX /O X n s - l o a q v o o 'p * a 'M SCZCOBS-'llB SPXXOX 6 6 /C t/O X n s -T 0 J 3 H 0 3 *pAa 'NSCZtO B6-'lX V 'SPXXOX quVTB H0*N 66/C X /O X 66/C X /O X 66/C X /O X 66/C X /O X 66/C X /O X 10 3003n s 'T -T X -iO 3 -q A d 0 S Z - 6 C X 0 im ns - X ' xAq 'N PC Z C O V l-lX a 03009ns -1 0 3 3 0 0 9 ' t / a 'KCCCC0B6-'UB ns - t X 'l A a 'NZCZC0B6-1XB SU - t 0 1 3 0 0 9 'l A a 'NXCZC0B6-'1XB ns -T 033O 09 * I^ a 'N0C5C0W6-1X3 'SPIXOX 'SPXXOX 'SPXXOX 'SPIXOX SPXXOX 'SPIXOX q u I 8 HO*K n s 'X X -qdd000X -6C X 0I*IBB 'SPXXOX 'n s 'x x - q < M o s i- 6 C i o i i a B s p ix o x n s 'X X -q ^ O O S -S C T O IlB B SPXXOX n s 'T i-q U o s z -e c io riB N ' spixox BBS 'T X - q * S 0 0 T - 6 C I 0 n B B 'SPIXOX n s * i i - q d A o s - 6 C i o n a B *s p ix o x n s 'ix-q<M sz~6C T on98 ' spixox n s * ix -q o i-6 C iO T * ia8 ' spixox n s 'T T -q * * s-6 C T o n a * ' spixox n s 'ii-q tt T B n A r i- 6 c t o n s B ' spixo x n s 'x x - q n x t o zH -6 C io n sB ' spixo x q u * t e HO*H q u o t a HO*N q u o t a HON 3KO* O tttO td N lo a P 9 0 6 6 S I0 I P9 C 9 0 6 6 S I0 I C9 Z 9 0 6 6 S I0 I 59 X 9066S I0I 19 09066ST0X 09 6S O 66S I0I 6S BS066STC! es 1 S 0 6 6 S T 0 I 1S 9SO66SI0I 95 S S O 6 6 S I0 I SS PS066STO I PS CS066ST0I cs Z S 0 6 6 S I0 I ZS ISO 66SI0I IS 0 S 0 6 6 S I 0 I OS 6P 066S I0I 69 B 9066SI0I 8P 1PO66SI0I IP 9P066S101 9P S P 0 6 6 S I0 I SP P P O 6 6 S I0 I PP C P 0 6 6 S I0 I CP Z P O 66S I0I 59 XPO66SI0I IP 0 P O 6 6 S I0 I OP 6C066SI01 6 C 8C066STOT fif 1C 0 6 6 S 1 01 1C 9C066SIOI 9 C SC066SIOI se PC066S10X PC C C 0 6 6 S I01 c t ZC066S101 z c IC 0 6 6 S I0 I IC O C 066S I0I OC 6Z066SX0I 65 9Z066SI0I 85 1Z066SI0I 5 9 5 0 6 6 S I0 I 95 S Z 0 6 6 S IO I SZ PZ066SIO I 95 CZ066SIOI tz ZZ066SI0I zz I5 0 6 6 S I0 I IZ 0 Z 0 6 6 S I0 I OZ 6I066ST0T 61 8 I0 6 6 S I0 I 81 1 I0 6 6 S I0 I 1 9 I0 6 6 S I0 I 91 SI066SIO I SI PX066SI0I PI C I0 6 6 S I0 I CI ZX066SI0I ZI II 0 6 6 5 I0 I XI 0I066SI0X 01 60066SI0I 6 80066S10I 8 10066SICI 1 90066SIO I 9 S0066SI01 S P0O66SI0I P C0066S10X t Z0066SIOX z I0066STOX I MON 9 (CUD) Y04< *-t p o n e tt e o <T 50*05:60 9X 390 VON p*3Ti :op9 q o r 666T TZ:t:0 9T 390 o* :pT3TPO* 3*<n ST0I\0W 3*\3d*a*3-dno\j0U'lfYK\:0 :poqaN 666T 0:t:0 91 390 d o n :poTJTPCw 3*oj M TO T\aT^*f\**'3O .*-d*w >0\uit8O t\:O :a r i 66/CX/OX *3X9 -OOOP poi 1093009 ` f 1 \ Avp '9**TT 303 S9TX0* 390dw Axoum e pmodtaoo XgtaaonO I 3337""'""--7 ' "S*S3 "77777 775373 3 373735 S|33733|3 77" " "'77S 53555333555 333335 S55555 5S55SS SSS5SS 553555553 553333555 c aaaaaaaaaaa aaaaaa aaaaaa aaaaaa a aaaaaa aaaaaaaaa aaaaaaaaa mmm mm mm mm =mm rm m i mmm3 nt Si o sS S slisssS s 533533 335335 i s s i l i 3 333333 335335=3 33 SSSSSSooo ope ttUUttUltU 5 5 5 5 5 5 555555553 O O 88 88 <r3> * 5 88 33333 3333 3SSSS 373V: 33333 3333 S HSSSSB Sigllg- l i * ..................... SB B I B B S i i l a B -fc B f? ? ? * m ; k k i i ........... C S| !gjII iIH=i5s-8S8a5 111 3 3 3 3 ? |3 3 J J I I I 5 3 | | | | 3 3 gBBSBSSS- 1 m um m I Sllii i P l IWIHI WWtNW S | | | a a a a a a a a a a a | a a a a 5 a | 5 5 5 a aSa 3| 5 5I l5l 5 aS a3 |aa |5a5a5a555aaa3|Sa | a 5a 5a 5a 2a |Sa | a a a ! " " "S3S3S33SS"3S3SS5*S5SS"SS5355"3"3353"" 33S3" 3*33S ......................................................'.."..."...".. .".."...".. 3l l33'3. 3 3 3 3 3 3 3 3 3 3 3 3 3 3 ..................... 333SS3S33S333SS3SSS3SS3SSSS3S3SS333SS3S3SSSSS53S3SSSS3SS3 333333533S3333SS53SS33333553S3333S353;S3535555S533 D 020199: Q u u e l f l*d u d prit*d by l u 10/19/99 D O oO __________________________________________________________________________________________________ f c / f r / f ? Quantify Calibration aapozt YOX14S- rat livor, day 1 4 4 , control and tea* ont. 10/13/ff , 7>- / < > / / * 9aa* 1 000698 Quantify Calibration M p o r t Y0X14S- rat livor, day 1 a 4, control and doaa- t . 10/13/9* t ago 2 000699 Quantify Calibration Xaport TOX145- rat livor, day 1 X 4 , control and dona- aact. 10/11/99 Vaga 3 000700 Quantify Calibration Ikaport 90X145- rat livor, day 1 a 4, control and tea- ext. 10/13/99 t Pag 4 000701 Method Report Method ile: Last modified: Compound: Printad: C: \MASSLYNX\soup-rats.pro\NethDBM01S99a.mdb Mon Oct 18 06:41:21 1999 1: POAA (Chi) Mon Oct 18 07:46:51 1999 Compound Heme: Zntarnal Ref.: Quantify Trace: Cone, of Standard: User RF Valua: User Paak Factor: Integrate Window Factor: Chromatogram m s a window: POAA (Chi) [Nona] TIC Cone. A 1.000000, Disabled 1.000000 2.000 l.QOOODa Retention Tina (mins): Relative Retention Tiae: RT Reference: Time Window (mins): Peak Selection: 7.129. tnabled 0.000, Disabled (None! 0.356 Nearest Response Type: External Polynomial type: Point of Origin: Fit weighting: Axis Traasfonation: units: Peak-to-peak amplitude: Smoothing: Window sire (scans): Number of smooths: Smoothing method: Join valley threshold: Reduce peak tailing: Raise baseline maximum: Draw vertical threshold: Detect shoulders: Shoulder threshold: Relative height: Absolute height: Relative area: Absolute area: Linear Exclude 1/X None 66 Enabled 2 1 30.00 200.00 9.00 90.00 Disabled 30.00 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled I t / n / r f j>OZot71 000702 N t M d Rapare Machad fila: beat nodified: Compound: Princad: C:\Mk5SLYBX\soup-rats.pro\MathDB\101599a.adb Moa Oet 18 04:41:21 1999 2 : p r o s (Ch2} Mon Oct 18 07:44:51 1999 Coapeund Maata: Internal Raf.: Quantify Trace: Cone, of Standarda: Oaar ftp Vala: Deer Paak Factor: Integrate Window Factor: Chroaetograa nans window: PPOS <Ch2) fMone) TIC Cone. R 1.000000. Diaablad 1.000000 2.000 l.OOOODa Ratantion Tine (nina): Ralativa Ratantion Tiste; RT Rafaranca: T i m window (mins): Paak Salaction: 7.311. tnablad 0.000. Diaablad [Mona) 0.400 Raapoaaa Typa: Raaponaa: external Amt Polynomial Typa: Point of Origin: Pit Kaightiag: Axis Transformation: Linear Zxclude 1/X Mona Onita: Peak-to-paak amplitude: (6 Smoothing: Window aisa (acana): Huatbar of smooths: Smoothing method: Enabled 2 1 Join vallay thraahold: Raduca paak tailing: Raiaa baaalina mart want: 30.00 200.00 5.00 Draw vartical thraahold: Dataet ahouldara: Shouldar thraahold: 90.00 Diaablad 30.00 Ralativa haight: Absolute haight: Ralativa araa: Absolute araa: 1.S0, Disabled 0.00. Diaablad 2.00. Disabled 0.00, Disabled uk Paso 2 000703 Method Report Method file: Last oditied: C :\MASSLYNX\soup-rats.pro\MethDBU01S99a.db Hon Oct 18 06:41:21 1999 ' Coepound: 3: PFOSA (Ch3) Printed: 001 " 7:,t:51 w>_______________________________________ 5 1 ^ 0**17* Coapound Name: Internal Ref.: Quantify Trace: Cone, of Standard: PPFroOSSAA <(CChh33)) (None) TIC Cone. C ' User RP Value: User Peak Factor: Integrate Window Factor: Chromatogram mass window: 1.000000, Disabled 1.000000 2.000 1.00000a Retention Time (ados] ; Relative Retention Time: RT Reference: Time Window (mins) : Peak Selection: 7.797, enabled 0.000, Disabled (None) 0.679 nearest Response Type: Response: External Areas Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Linear Exclude l/X Nona Units: Peak-to-peak amplitude: 60 Smoothing: Window sire (scans): Humber of smooths: Smoothing method: Enabled 2 1 Join valley threshold: Reduce peak tailing: Raise baseline aaxiaum: 30.00 200.00 S.00 Draw vertical threshold: Detect shoulders: Shoulder threshold: 90.00 Disabled 30.00 Relative height: Absolute height: Relative area: Absolute area: 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled Page 3 >*frgji* 000704 Method Report Matbod fila: Last modified: Cesqpound: Printed: C:\MASSLYNX\soup-rata.pro\NathDB\101S99a.mdb Mon Oct 16 06:41:21 199 4: IS (Ch4) Moa Oct 18 07:46:51 1999 Compound Nana: lotaraal Ra.: Ooantify Traca: Coac. of Standards: Uaar RP Vala: User Peak Factor: integrate Window Factor: Chroaatograa maas window: ZS (Ch4> {Nona] TIC Fixed 1.000000. Disabled 1.000000 2.000 l.OOOODa Ratantion Tina (ados): Relativa Retention Ti RT Ra{arance: Tine Window (ana) : Peak Selection: 7.157. Enabled 0.000, Disabled (Nona] 0.411 Nearest Rasponea Type : Response : External Areas Polynomial Type: Point of Origin: Pit Weighting: Axis Transformation: onits: Linear Exclude l/x Nona Peak-to-peak solitude: 67 toothing: Window sisa (scans): Number of smooths: Smoothing matbod: Enabled 2 l Join valley threshold: Reduce peak tailing: Raise baseline maxisum: 10.00 200.00 5.00 Draw vertical threshold: Detect shoulders: Shoulder threshold: 90.00 Disabled 30.00 Relative height: Absolute height: Relative area: Absolute area: 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled 2*T*t1 Page 4 000705 Q uattro II, #6414E SOUP 020199: FACT Equipment Log 99092 PAGE 1/1 DATE: 10/15/99 ANALYST:ias STUDY NUMBER: TOX145 MATRIX: rat liver DESCRIPTION:davs 1&4 FACT Method: ETS-8-7.0 Injection volume: 10 uL Cycle time: 10 min. Electrode: Z-Sprav Mobile Phase: (A12.0 mM NH4CH3CQ2 (B).MsQH TN-A- or stndrd number (A) 99085-10-5________ (B) TN-A-2878 Prepared (date/by): (A) 10/10/99 sah________ (B) 10/10/99 1. Expires: (A) 04/00______________ IB) 2010______ Store at room temp? @ or N Other:_ G uard column: None__________________ Part number: na_________ Lot number: na Analytical column: Keystone Betasil____________________________________ Size: 2 x 50 mm________________ Type: C lg___________ Sphere sizeijLnm______ Part number: 055-701-2__________ Lot number: P9E11 Serial number:0591804Z Analytical parameters: Drying gas (L/hri: 350 ESI nebulizing gas IL/hr) 13 LC Flow rate: 300 uL/min. Back pressure: 65 bar Sheath gas (L/hr)_Q. HPLC solvent gradient: 10min-10-95 Time (min .)____ DJLQ__________ 2LLQQ________ 3) _L2fl______ 4 ) 7.50 5 1M Q ________ JM M 3S& 2LQ_ 1Q JL 000706 Tuning Method Report Method: C :\MASSLYNX\SOTJP-RATS.PR0\ACQUDB\PF0S3 Printed: Fri Oct 15 11:42:32 1999 Page 1 SOURCE ( ESP- ) CapillaryCone Extractor RF Lens Source Block Temp. Desolvation Temp. Set Rdbk 3.00 40 5 0.2 150 250 3.00 -41 -6 153 250 Pressures Analyser Vacuum Gas Cell Rdbk 6.6e-5 4 . le-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set 14.0 14.0 0.9 0.0 4 650 Set RdQ 14.0 14.0 10 2.0 0.0 40 0 650 7 38 -0 Method: c: \k o s i t m x \s o o p -i u t s .rnovacgotuvioicxii-pro*-eoju-proaa-xs L u t Modified: Fri Oct 15 11:35:03 1999 matad: rrl Oct 15 11:42:4 199 Solvent Delay ( alas ) ! 0.00 Function : 1 M U of 1 Mass Pair ( BSP- ) Inter Channel Delay I[ Secs ) : Span < Daltons > ; Start T i m ( Mins ) : Bnd T i m < Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) Coll Bnergy (eV) Cone 1 413.00 1C9.00 0.30 30 15 Function : 2 1001 of 1 Mana Fair { U P * ) Inter Channel Delay ( Seca ) : 0.03 Span { Daltone ) : 0.00 Start T i m < Mina > : 0.00 Bad T i m { Kina ) : 10.00 Repeats : 1 Channel Parent Daughter Dwell (Secs) Coll Baergy (eV) Cone ( V ) 1 499.00 99.00 0.30 45 CO Function : 3 MRN of 1 Maas Pair ( BSP- ) Inter Channel Delay < Soca ) : Span ( Daltons ) : Start T i m ( Min* ) : Bad Ti* ( Mina ) i Repeats : Channel Parent Daughter 0.03 0 .0 0 0.00 1 0 .0 0 1 Dwell (Secs) Coll Bnergy (eV) 1 498.00 78.00 0.30 43 Cone ( V } CO Function : 4 of 1 Pair ( BSP- > Inter Channel Delay ( Secs ) : Span ( Daltons ) : Start T i m ( Kins ) : Bnd T i m ( Kins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Sees) Coll Bnergy (ev> 1 427.00 80.00 0.30 40 Cone ( V ) 80 Page 1 000708 IHthed Report Method rile: Last Modified: Printed: C: \MASSLYX\30r-RATB.PRO\ACQOTB\10min-10-95 Friday, October IS, 1999 11:43:04 Friday, October 15, 1999 11:43:13 HP1100 LC Pun Initial Cooditiona Solvents A% B% C% D% 90.0 10.0 0.0 0 .0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 0.300 10.0 0 400 30.0 30.0 HP1100 LC Pus gradient Tijeetable The gradient Timetable contains 5 entries which are : Time At B% Ct D% 0.00 90.0 10.0 0.0 0.0 1.00 90.0 10.0 0.0 0.0 5.50 5.0 95.0 0.0 0.0 7.50 5.0 95.0 0.0 0.0 8.00 90.0 10.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 BP1100 LC Puap External event Timetable The Timetable contains 3 entries which are : Time Initial 0.00 0.10 Column Switch Contactl Off Off Off On Off Off Contact2 Off On Off Contact3 Off Off Off Contact4 Off On Off HP1100 Rutoeanpler Initial Conditiona Draw Speed Eject Speed (pl/min) Draw Position (mm) Stop Time (mins) Injection Volume(ul) Vial Number 200.0 200 0.00 9.00 5.0 91 400 400 400 400 400 Masslynx - Sample L itt Sample List: C:\MASSLYNX\soup-rats.pro\SampleDB\101599a.SPL Printed: Fri Oct 15 11:56:25 1999 Page Position: (1 ,1 ) File Name File Text MS File 1 101599001 M eOH Blank 10M IN -P F O S -P O A A -P F O S A -IS 2 101599002 MeOH Blank 10M IN -P F O S -P O A A -P F O S A -IS 3 101599003 MeOH Blank 10M IN -P F O S -P O A A -P F O S A -IS 4 101599004 T O X 1 45, R BL10 1 3 9 -H 2 0 Blank-11, S EE 10M IN -PFO S-PO A A -PFO SA -IS 5 101599005 TO X145, RBL10139-Uver Blank-11, SEE 6 101599006 T O X 1 45, RBL10 1 39-5p pb-11, S E E 10M IN -PFO S-PO A A -PFO SA -IS 10M IN -PFO S-PO A A -PFO SA -IS 7 101599007 TO X145, RBL10139-10ppb-11. SEE 10M IN-PFO S-PO AA-PFO SA-IS 8 101599008 TO X145, RBL10139-25ppb-11, SEE 10M IN -PFO S-PO A A -PFO SA -IS 9 101599009 TO X145, RBL10139-50ppb-11, SEE 10M IN -PFO S-PO A A -PFO SA -IS 10 101599010 T O X 1 45, R BL101 3 9 -1 00ppb -11, SEE 10M IN -P F O S -P O A A -P F O S A -IS 11 101599011 T O X 1 45, R BL10 1 39-250pp b-11, SEE 10M IN -PFO S-PO A A -PFO SA -IS 12 101599012 T O X 1 45, R B L10139-500pp b-11, SEE 10M IN -P F O S -P O A A -P F O S A -IS 13 101599013 TO X145, RBL10139-750ppb-11, SEE 10M IN -P F O S -P O A A -P F O S A -IS 14 101599014 T O X 1 45, R B L10139-1000p pb-11, S EE 10M IN -PFO S-PO A A -PFO SA -IS 15 101599015 M eO H Blank 10M IN -P F O S -P O A A -P F O S A -IS 16 101599016 T O X 1 45, R TL -9R 03 230 M , D y l, Control- S E E 10/13/99 10M IN -P F O S -P O A A -P F O S A -IS 17 101599017 T O X 1 4 5 , R T L -9R 03231M , D y l, Control- S E E 10/13/99 10M IN -P F O S -P O A A -P F O S A -IS 18 101599018 TO X145, RTL-9R 03232M , Dy1, Control- SEE 10/13/99 10M IN -PFO S-PO A A -PFO SA -IS 19 101599019 T O X 1 4 5 , R TL -9R 03 233 M , D y l, Control- S E E 10/13/99 10M IN -P F O S -P O A A -P F O S A -IS 20 101599020 T O X 1 4 5 , R T L -9R 03234M , Dy1, Control- S E E 10/13/99 10M IN -P F O S -P O A A -P F O S A -IS 21 101599021 T O X 1 45, RBL10 1 39 -250 p p b -C C V -11-1, S EE 10M IN -P F O S -P O A A -P F O S A -IS 22 101599022 M eOH Blank 10M IN-PFO S-PO AA-PFO SA-IS 23 101599023 TO X145. RTL-9R 03235M , Dy4, Control- SEE 10/13/99 10M IN -P FO S -P O A A -P FO S A -IS 24 101599024 T O X 1 45, R TL -9R 03 236 M , Dy4, Control- S E E 10/13/99 10M IN -P F O S -P O A A -P F O S A -IS 25 101599025 TO X145, RTL-9R 03237M , Dy4, Control- SEE 10/13/99 10M IN -PFO S-PO A A -PFO SA -IS 26 101599026 T O X 1 45, R TL -9R 03 238 M , Dy4, Control- S E E 10/13/99 10M IN -P F O S -P O A A -P F O S A -IS 27 101599027 T O X 1 45, R TL -9R 03 239 M , Dy4, Control- S E E 10/13/99 10M IN -P F O S -P O A A -P F O S A -IS 28 101599028 T O X 1 45, R BL10 1 39-250 p p b -C C V -11-2, SEE 10M IN -P F O S -P O A A -P F O S A -IS 29 101599029 M eO H Blank 10M IN-PFO S-PO AA-PFO SA-IS 30 101599030 TO X145, 9R 03230M , Dy1, Control-250pb-MS-11 10M IN-PFO S-PO AA-PFO SA-IS 31 101599031 T O X 1 45, 9 R 03 230 M , D y1, Control-250pb-M SD -11 10 M IN -P F O S -P O A A -P F O S A -IS 32 101599032 T O X 1 45, 9 R 03 235 M , Dy4, Control-250pb-M S-12 10M IN-PFO S-PO AA-PFO SA-IS 33 101599033 TO X145, 9R03235M , Dy4, Control-250pb-MSD-12 10M IN -P F O S -P O A A -P F O S A -IS 34 101599034 T O X 1 45 , R TL -9R 03 245 M , D y l, 5m g/kg- S E E 10/13/99 10M IN -P F O S -P O A A -P F O S A -IS 35 101599035 T O X 1 45 , R BL10 1 39 -250 p p b -C C V -11-3, SEE 10M IN -P F O S -P O A A -P F O S A -IS 36 101599036 M eO H Blank 10M IN-PFO S-PO AA-PFO SA-IS 37 101599037 TO X145, RBL10139-250ppb-CCV-11-3, SEE 10M IN-PFO S-PO AA-PFO SA-IS 38 101599038 M eO H Blank 10M IN -P F O S -P O A A -P F O S A -IS 39 101599039 TO X145, RTL-9R 03246M , Dy1, 5mg/kg- SEE 10/13/99 10M IN-PFO S-PO A A -PFO SA -IS 40 101599040 T O X 1 45, R TL -9R 03 247 M , D y l, 5mg/kg- S E E 10/13/99 10M IN -P F O S -P O A A -P F O S A -IS 41 101599041 T O X 1 45, R TL -9R 03 248 M , D y l, 5mg/kg- S E E 10/13/99 10M IN -P F O S -P O A A -P F O S A -IS 42 10 1599042 T O X I45, R T L -9R 03249M , D y l, 5m g/kg- S E E 10/13/99 10M IN -P F O S -P O A A -P F O S A -IS 43 101599043 TO X145, RTL-9R 03250M , Dy4, 5mg/kg- SEE 10/13/99 10M IN-PFO S-PO A A -PFO SA -IS 44 101599044 TO X 145, RBL10139-250ppb-CCV-11-4, SEE 10M IN-PFO S-PO AA-PFO SA-IS 45 101599045 M eO H Blank 10M IN -PFO S-PO A A -PFO SA -IS 46 101599046 T O X 1 45, R BL10 1 39 -250 p p b -C C V -11-4, SEE 10M IN -PFO S-PO A A -PFO SA -IS 47 101599047 M eO H Blank 10M IN -PFO S-PO A A -PFO SA -IS 48 101599048 TO X145, RTL-9R 03251M , Dy4, 5mg/kg- SEE 10/13/99 10M IN -PFO S-PO A A -PFO SA -IS 49 101599049 TO X 145, R TL-9R 03252M , Dy4, 5mg/kg- SEE 10/13/99 10M IN -PFO S-PO A A -PFO SA -IS 50 101599050 TO X145, RTL-9R03253M , Dy4, 5mg/kg- SEE 10/13/99 10M IN -PFO S-PO A A -PFO SA -IS 51 101599051 T O X 1 45, R TL -9R 03 254 M , Dy4, 5mg/kg- S E E 10/13/99 10M IN -P F O S -P O A A -P F O S A -IS 52 101599052 TO X145, RBL10139-250ppb-CCV-11-4, SEE 10M IN-PFO S-PO AA-PFO SA-IS 53 101599053 M eO H Blank 10M IN -P F O S -P O A A -P F O S A -IS 54 101599054 T O X 1 45, R B L10 1 39 -250 p p b -C C V -11-4, S EE 10M IN-PFO S-PO AA-PFO SA-IS 55 101599055 M eO H Blank 10M IN-PFO S-PO AA-PFO SA-IS 56 101599056 T O X 1 45. R BL10 1 39-5p pb-11, S EE 10M IN-PFO S-PO AA-PFO SA-IS 57 101599057 TO X145, RBL10139-10ppb-11, SEE 10M IN-PFO S-PO AA-PFO SA-IS 58 101599058 TO X145, RBL10139-25ppb-11, SEE 10M IN -P F O S -P O A A -P F O S A -IS 59 101599059 TO X145, RBL10139-50ppb-11, SEE 10M IN-PFO S-PO AA-PFO SA-IS 000710 Masslynx Sample List Sample List: C:\MASSLYNX\soup-rats.pro\SampleDBVI 01599a.SPL Printed: Fri Oct 15 11:56:25 1999 Inlet File Bottle Inject Volum e Sam ple Type Cone 1 10m in-10-95 91 2 10m in-10-95 91 3 10m in-10-95 91 4 10min-10-95 1 5 10min-10-95 2 6 10min-10-95 3 7 10min-10-95 4 8 10min-10-95 5 9 10mirt-10-95 6 10 10min-10-95 7 11 10m in-10-95 8 12 10min-10-95 9 13 10min-10-95 10 14 10m in-10-95 11 15 10min-10-95 92 16 10min-10-95 12 17 10min-10-95 13 18 10min-10-95 14 19 10min-10-95 15 20 10min-1O-95 16 21 10m in-10-95 36 22 10min-10-95 92 23 10min-10-95 17 24 10min-10-95 18 25 10min-10-95 19 26 10min-10-95 20 27 10m in-10-95 21 28 10min-10-95 37 29 10min-10-95 93 30 10min-10-95 22 31 10m in-10-95 23 32 10min-10-95 24 33 10min-10-95 25 34 10min-10-95 26 35 10min-10-95 38 36 10min-10-95 93 37 10min-10-95 38 38 10min-10-95 93 39 10min-10-95 27 40 10min-10-95 28 41 10m in-10-95 29 42 10min-10-95 30 43 10m in-10-95 31 44 10min-10-95 39 45 10min-10-95 94 46 10min-10-95 39 47 10min-10-95 94 48 10min-10-95 32 49 10min-10-95 33 50 10min-10-95 34 51 10m in-10-95 35 52 10min-10-95 39 53 10min-10-95 95 54 10min-10-95 39 55 10min-10-95 95 56 10min-10-95 3 57 10min-10-95 4 58 10min-10-95 5 59 10min-10-95 6 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 .10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 _ -- -- -- -- -- ---- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- ___ -- -- ___ -- -- -- -- -- ___ -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- ___ -- -- -- ___ ___ -- ___ ___ ... -- -- -- ___ -- -- Page 2 Page Position: (2 ,1 ) 000711 M asslynx - Sam ple U e t Sample List: C:\MASSLYNX\soup-rats.pro\Sam pleDB\101599a.SPL Printed: Fri Oct 15 11:56:26 1999 Page 3 Page Position: (1 ,2 ) File Name File Text 60 101599060 TO X145, RBL10139-100ppb-11, SEE 61 101599061 T O X 1 4 5 , R B L10 1 39 *25 0p p b -11, S E E 62 101599062 TO X145, RBL10139-500ppb-11, SEE 63 101599063 TO X145, RBL10139-750ppb-11, SEE 64 101599064 TO X145, RBL10139-1000ppb-11, SEE M S File 10M IN-PFOS-POAA-PFOSA-IS 10M IN -P FO S -P O A A -P FO S A -IS 10M IN-PFOS-POAA-PFOSA-IS 10M IN-PFOS-POAA-PFOSA-IS 10M IN -P FO S -P O A A -P FO S A -IS / 000712 Masalynx Sample List Sample List: C:\MASSLYNX\soup-rats.pro\SampieDB\101599a.SPL Printed: Fri Oct 15 11:56:26 1999 Inlet Hie Bottle Inject Volume Sample Type Cone A 60 10min-10-95 7 61 10m in-10-95 8 62 10min-10-95 9 63 10m in-10-95 10 64 10m in-10-95 11 10.000 10.000 10.000 10.000 10.000 -- -- -- -- -- -- -- -- -- Page 4 Page Position: (2, 2) 000713 FACT: DATA REVIEW SUMMARY FORM Date: Data Analyst: FACT Study #: Matrix/Timepoints: /< T _ r , /? . Sample List Set-up Analysis Date/Analyst: /0 '/9 - ^ 7 Instrument: J ^ i2 2 /A 4 ^ d l a ^ jL Analyte: _ ~>PT& Acce^aUeUnevRuge: f) sy-l--\ LOQ: Extraction Blank: i f i . TC /O - Q f f i ? ______ Matrix Blank: c ' / ' L L o a Calibration Checks: _______________________________________ MS/MSD:___________ 0 | _______________________________ Data Status:a n k rttl UC Analyte: Acceptable Linear Range: LOQ: / . t f A f p Jc> R-2: /)> Extracted Blank: fa fjb Q L . Matrix Blank: ^ ^ 3 . L O Q ^ Calibration Checks: M S /M S D :____ Data Status;S . &-- J2L tn \(M U \ L Id I i x K i Data ReviewSign-OfT Technical Review Nam e/ Date: . . /. i a / ^ o M j tyh /Q/&/3 Quality Assurance Review Name / Date:_____________ D ata E n try :__ LAc Comments / Justiflcatkms: ip h i)q q -So-29f -k> Miei/- &%Xt//<z)r) r/t>7G-, < 3 l _ m - W S a >o-r ~77*r /nu6*> y.J Pom U f ^ fJoT-atli-Sefi "T E fe te * 1^ Ac/kTVr,______ 0i.^A~yOLe. / v o - r _______ / W t / a / J^7TpeA/Ac. oe , SPr~y>u?T. wots-e2xAA*rr,-mr<ph .r e jt*J Analyte: > 9 - ( J ) Acceptable Linear Ranse: ~w LOO: ------- Extracted Blank: R-': ' Matrix Blank: Calibration Checks: MS/MSD. " ________ Data Satas: e r t / / - h # M k r u z A /yrf--/rr ~ 000714 FACT: DATA REVIEW SUMMARY FORM Date: Data Analyst: FACT Study#: ' To y Matrix/Timepoints: Sample Lilt: Set-up Analysis Date/Analyst Instrument mW / in u ________ _______ Data Review Sign-Off Z Z S r J n f o .A r jt& 7 Technical Review p \ I f0 Name/Date: \L > W H p ^jL I Ot J - U 6 Quality Assurance Review Name >Date: __________________________________ Data E n try :___ U l loh t-h i A n alyte:. Acceptable Linear Range: LOQ:_________ *-------- ` RA2 :_________ Calibration Checks: M S /M S D :_______ Data Status:______ Extraction Blank:. Matrix Blank: 000715 * e t S i 9 S I 000716  s t : s s : ! ; s s g ! S 3 S S 2 i ; K ; s : : t : s n : : t : ! : t : s , . - . , u.-o ,K .^ - ooooooooooooooooooooooooooooooooooooooof llllilllllliiil sgsssfssssa|fsssssisrssssisss^sssssssli( S S S S S S p S H SSSSSS 5SSSS 5SSSS5S555S | mmurnmrmnmmmm mmmm mmummmm ? I pigg|K|pg m u 2IIII pISIsr |p i ffwle? im flhi lC r r - r - tc r c "" * "" ' ? s c s c r r r ' f s Lr IHi;ii?as! bI8Ss#iW i!!!!:!S"K!?:! ,, ,,ooooo SooooiiiC -? G iP H *| i i t m m f E IH li P s> I S S 3 S 2 - ggggSSSS i g s s s s s :,.. ggggsk'skis - S5S=S=SiSHSSSSS==S=55S555SSS=y5i55=555s ja 7*> 5 I I ~ S 2 = S: J I S SS ^ & & siss=oooooS5s252oiS5SsSo"5sSsss,,ooooog SSSSSSggggggSISSSg5SSSSgSc!S5gggggg? <*>3 i S g f g i S m S g S i S * m ? i i i i g | 5 g ? & | Il I I # II-*- oI il u>OHMIeHwNoOoOo I 4M I iH iI^IHH*NoHu * y ooHoHO p <i o! Q? J -X>  K ee ! e c i i 9 9 1 000717 sssgssBBsgssasssKSitisgssssscKss,...,........^-. z-Ar- i 223SsHHBiliSsSsiHsisSIsHsHHsilsS2222ssl llllilillilllll ssssasssssBassssssssssssssssssssss| 3 ? ? UUU UMUU 1 sr I ili i ! j:??????? ? IP P P * s p l i l l " " 1 1 1 " s ls l"% " g ||||| s u m s ls l: ; : |l J r liiiiHI HliUI s S E S r r r * T p *** s s s s r r r * T" ? H & g 5 R R B RSR B ,,9OODDO ,,O1O8OOD s 5BBr B " " ^ b 3 " h 5 Rggggg Rggg g l " s s s s ? ? ? Rs W m % p wmK s s. 5= S S SS S .. gg'ggkggbs s g I li g'gggks's - " I 5 s i " g" 5 = I *g 5 K s is i= K 5 " Bl f l l i S S s s g B s S s I S S . I I I I I s g l l s l SSSSSf i 2gSgSSS,,*-^oS523og5SgSSoSSSS.-oooog 2 gigggsssgbsgksssssgbkskkiibgssbbgibskggp gim m gm sggsm sissH gggism issm ? J .. ^ gs,,2gi - + ,. . - , ggis: lH Qj?> _rC m v> T-> -- I> ! M r K 0 s w !t s 1 i J*a* l 9 I 00071S ssassssssiSKSBrSss 2222222222222222223222 liiililil! 8 S S 8 8 ? 8 S S S S S ? K * IS S S S S S S S S ? S S 1 ? 1 oS' -t- ci n p 5 D* dT sssssssss r ~> T S53SSS2SSSS *22252 n**u sssssssss 25222IS22I5 s ! 5 issss;S K S S S S i B S S S SSSBS2 SSSSSS <-> 1 S~ SSSSCSBSaSB SSSSSB S2X2S B S S S 3 S 2 S S S 2 SSSSSSS5SSS & S S m ms&g S&ggS&S&g s: o Itili SS.erBBSS.B i ; i ; - . , > , 2 ? 1 ! --A Quantify Cca^ound I Tox 145: Rat laaaii Dilubtane, Day 1,4 Saaple List: C:\MkU0ntic\aMa4a-rmte.fRO\SaapleOR\lO1999a Last aodified: Mad Oet 30 00:31:4? 100 Method: C :\MRSSLTKX\naelie-reta. PRO\MethDB\101999a Last aodifiad: ad Oet 20 00:14:10 100 Job Coda: Printed; Oad Oet 30 00:00:41 1000 Compound 4 : IS (Ch2) Mane 1 101990001 2 101990002 3 101999003 4 101999004 S 101999005 6 101999006 7 101999007 8 101999008 9 101999009 10 101999010 11 101999011 12 101999012 13 101999013 14 101999014 IS 101999015 16 101999016 17 101999017 10 101999018 19 101999019 20 101999020 21 101999021 22 101999022 23 101999023 24 101999024 2S 101999025 26 101999026 2 7 101999027 28 101999028 29 101999029 30 101999030 31 101999031 32 101999032 33 101999033 34 101999034 35 101999035 36 101999036 37 101999037 38 101999038 39 101999039 Saapleliat fast MeOH KaOH Tox 14S: RBL10139-H20 blk-ll, Ext SEE 10-13-99 Tox 145: RBL10139-Liver blk-11. Ext SEE 10-13-99 Tox 145: RBL10139-5 p p b-U, Ext SEE 10-13-99 Tox 145: RBL10139-10 p pb- U , Ext SEE 10-13-99 Tox 145: RBL10139-2S p pb- U , Ext SEE 10-13-99 Tox 145: RBL10139-S0 ppb-ll. Ext SEE 10-13-99 Tox 145: RB110139-100 p p b-U, Ext SEE 10-13-99 Tox 145: RBL10139-250 p p b-U, Ext SEE 10-13-99 Tox 145: RBL10139-500 ppb-ll. Ext SEE 10-13-99 Tox 145: RSL10139-750 p p b-U, Ext SEE 10-13-99 Tox 145: RBL10139-1000 p p b-U, Ext SEE 10-13-99 MaOH Tox 145: 9903237K, Day 4, Control, D:100 Tox 145: 9R0324SH, Day 1, 5 m q / k q , D:100 Tox 145: 9R03244K# Day 1, 5 m q / k q , D:100 Tox 143: 9R03247M, Day 1, 5 m q / k q , D:100 Tox 145: 9R0324M Day 1, 5 m q / k q , D:10O Tox 145: RSL10139-250 ppb-U-2, Ext SEE 10-13-99 MOH Tox 145: 9R03249K, Day 1, 5 m q / k q , D:100 Tox 145: 9R03251M, Day 4, 5 m q / k q , D:100 Tox 145: 9R03252K, Day 4, 5 m q / k q , D:100 Tox 145: 9R03253M, Day 4, 5 m q / k q , D:100 Tox 145: 9R03254M* Day 4, 5 m q / k q , D:100 Tox 145: RBL10139-2S0 ppb-U-1, Ext SEE 10-13-99 MaOH Tox 145: RBL10139-H20 blk-11, Ext SEE 10-13-99 Tox 143: RBL1Q139-Liver b l k - U , Ext SEE 10-13-99 Tox 145: R8L10139-5 ppb-U, Ext SEE 10-13-99 Tox 145: RBL10139-10 p pb- U , Ext SEC 10-13-99 Tox 145: RBL10139-25 p pb- U , Ext SEE 10-13-99 Tox 145: R8L10139-50 p pb-U. Ext SEE 10-13-99 Tox 145: RBL10139-100 p p b-U, Ext SEE 10-13-99 Tox 145: RBL10139-250 p p b-U. Ext SEC 10-13-99 Tox 145: RBL10139-500 p p b - U , Ext SEE 10-13-99 Tox 145: RBL10139-750 p p b-U, Ext SEE 10-13-99 Tox 145: RBL10139-1000 p p b-U, Ext SEE 10-13-99 Standard Standard Standard Standard Standard Standard Standard Standard Standard 0c oc Standard Standard Standard Standard Standard Standard Standard Standard Standard Std Cone 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 RT 6.982 6.955 6.961 6.956 6.958 6.951 6.960 6.956 6.957 6.938 6.934 6.957 6.976 6.980 6.970 6.955 6.904 6.984 6.961 6.902 6.960 6.903 6.960 6.900 7.007 7.003 6.979 6.956 6.987 6.963 6.959 6.958 6.957 6.961 6.955 (?) Aran Cone. Plaga %Dev 2946 3227 4774 4658 422? 4612 3958 4194 3767 3627 3291 30 36 43 34 32 2585 32 30 29 27 35 2759 9 2979 3288 3941 4386 4134 4085 3571 3937 3460 3218 3342 0.74 bb 0.81 bb 1.20 bb 1.22 bb 1.06 bb 1.16 bb 1.00 bb 1.05 bb 0.95 bb 0.96 bb 0.63 bb 0.01 bb 0.01 bd 0.01 bd 0.01 bd 0.01 bb 0.65 bb 0.01 bb 0.01 bb 0.01 bd 0.01 bd 0.01 bd 0.69 bb 0.00 bb 0.75 bb 0.83 bb 0.99 bb 1.10 bb 1.04 bb 1.03 bd 0.90 bb 0.99 bd 0.6? bb 0.61 bb 0.84 dd -26 -19 20 22 6 16 -0 5 -5 -4 -1? -99 -99 -99 -99 -99 -35 -99 -99 -99 -99 -99 -31 -100 -25 -17 -1 10 4 3 -10 -1 -13 -19 -16 Dla no)' uu A. l i a 042400: Quanti ta tad and P rin ted by a h 1 0/20/00 0007X 9 BEST COPY AVAILABLE Quantify Calibration tapert T a x 149: l U t ^ d t l T ^ i l y M b ^ a , Compouna 1 narnTPF OS Coefficient o f Determination: 0.989844 Calibration curve: 8.25151 * x + 352.987 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None ' - * > 9 9 ~ ^ /y 9ao 1 Aawlia 092499: Quantita tod and P rin ted by a * 1 0 /2 0 /9 9 000720 b e s t c o p y a v a il a b l e A M lla 0C24M: Q o M tltsta d and r la ta d by m * 1 0 /2 0 / 000721 Q u a n tify C a lib r a tio n Ha p e r t Tox 145: l u e ^ f f i r ^ D ^ k y o n i , Day 1 .4 Compound 3 name: POA Pa9* 3 Aaalia 024M: Quantitated and Printed by aah 10/20/M 000722 Q uantify c a lib ra tio n import To* 14S: Rat donar-D i n d o n a , Day 1,4 C om p o u n d ^n w n :IS (Ch2) ` Papo 4 I Aaolia 0434ft: Quantitt! and Printod by aatfi lO/30/tt 000723 Method Report Method file: U s t edified: Compound: Printed: N:\amalie- rats.PRO\MethDB\101999a.mdb Med Oct 20 01:14:11 19990 1: PFOS Thu Oct 2i 15:13:1? 1999 Co*pound Name: Internal Ref.: Quantify Trace: Cone, of Standards: User RF Value: User Peak Factor: Integrate Window Factor: Chromatogram mass window: Peak Location Retention Tine (mins): Relative Retention Time: RT Reference: Time Window (mins): Peak Selection: Response Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: Fie Weighting: Axis Transformation: Concentration Units: Noise Peak-to-peak amplitude: Smooth Smoothing: Window size (scans): Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: Peak Seoaration Draw vertical threshold: Detect shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative area: Absolute area: PFOS (None] TIC Cone. A 1.000000, Disabled 1.000000 2.000 l.OOOODa 7.16? Enabled 0.000, Disabled (Hone] 0.358 Nearest External Areas Linear Exclude l/x Moa* 100 Enabled 2 1 30.00 200.00 5.00 90.00 Disabled 30.00 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled t y Page i 000724 Method Report Method file: Laat Modified: Compound: Printed: N:\amelia- rats.PRO\MethDM\101999a.mdb Med Oct 20 09:19:19 19990 2: PFOSA Thu Oct 21 1$:13:19 1999 Compound Name: Internal Ref.: Quantify Trace: Cone, of Standards: User RP Value: User Peak Faetor: Integrate Window Factor: Chromatogram mass window: Peak Location Retention Time Imlns): Relative Retention Time: RT Reference: Time Window (mins): Peak Selection: Response Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Concentration Units: Noise Peak-to-peak amplitude: Smooth Smoothing: Window sire (scans): Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: Peak Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative ares: Absolute area: PFOSA [None] TIC Cone. B 1.000000, Disabled 1.000000 2.000 l.OOOODs 7.924, enabled 0.000, Disabled [None] 0.292 nearest External Areas Linear Exclude l/X None 94 Enabled 2 1 30.00 200.00 5.00 90.00 Disabled 30.00 1.SO, Disabled 0.00, Disabled 2.00. Disabled 0.00, Disabled (A m tfo u tta W f' Page 2 000725 Method Report Method iti; Lest modified: Compound: Printed: H : \ e m e i ie-tats.P A O \ H a t h o e U O l 9 9 9 a . m d b Ned Oct 20 01:16:16 1991G 3: POAA Thu Oct 21 15:13:11 1999 Compound Name! Internal Ref.: Quantify Trace: Cone, of Standards: User RP Value: User Peak Psctor: Integrate Window rector: Chromatogram suss window: Peak Location Retention Tine (mins): Relative Retention Tine: RT Reference: Tiae Window tains): Peak Selection: Response Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: Tit weighting: Axis Transformation: Concsntrstion POAA (None) TIC Pixed 1.000000, Disabled 1.000000 2.000 l.OOOODa 6.947, Enabled 0.000, Disabled (None] 0.231 Nearest External Areas Linear Exclude 1/X Peak-to-peak amplitude: Saooth Smoothing: Window size (scans): Number of smooths: Smoothing method : Baselines Join valley threshold: Reduce peek tailing: Raise basaline maximum: Peak Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative area: Absolute area: Enabled 2 1 30.00 200.00 S.00 90.00 Disabled 30.00 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled M i* , h '/tf /f M . ^ Page 3 0C0726 5 Method Report Method file: Lett modified: Compound: Printed: N:\amelia-rats.PAO\MathDS\101999a.mdb Ned Oct 20 09:16:19 1999C 4: 15 (Ch2) Thu Oct 21 15:13:19 1999 Compound Name: Internal Ref.: Quantify Trace: Cone, of Standards: User RF Value: User Peat Factor: Integrate Window Factor: Chromatogram m s s window: Peak Location Retention Time (tins): Relative Retention Tlae: RT Reference: Tlae Nlndow (ains): Peak Selection: Resoonse Response Type: Response: Calibration Curves Polynoaisl Type: Point of Origin: Tit Weighting: Axis Transforaation: Concentration Units: Noise Peak-to-peak amplitude: Smooth Smoothing: Window sire (scans): Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: Peak Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative area: Absolute area: IS (Ch2) (None) TIC Fixed 1.000000, Disabled 1.000000 2.000 1.00000a 9.910, Enabled 0.000, Disabled (None) 0.406 Nearest External Areas Linear Exclude 1/X None 94 Enabled 2 1 30.00 200.00 5.00 90.00 Disabled 30.00 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled \ Page 4 000727 AMELIA 062498: FACT Equipment Log ,99114 Q uattro n , #6448E PAGE DATE: 10/19/99 ANALYST: minh STUDY NUMBER:TOX145 MATRIX: rat liver DESCRIPTION: dil FACT Method: ETS-8-7.0 Injection volume: 10 uL Cycle time: 10 min. Electrode: Z-Spray MobUe Phase: (A)2.0 mM NH4CH3C02 TN-A- or stndrd number (A) 99085-10-14______ (B) MeOH (B) TN-A-2997 Prepared (date/by): Expires: (A) 10/16/99 sah_______ (A) 04/00 (B) 10/16/99 sah (B) 04/00 Store at room temp? 0 or N Other:__ G uard column: None__________________ Part number: na_________ Lot number: na Analytical column: Keystone Bctasil____________________________________ Size: 2 x 50 mm________________ Type: C18___________ Sphere size: 5 um______ Part number: 055-701-2__________ Lot number: P9E11 Serial number:0591816Z Analytical parameters: Drying gas (L/hr): 300 ESI nebulizing gas (L/hr) 10 LC Flow rate: 300 uL/min. Back pressure: 62 bar Sheath gas (LVhr)_0 HPLC solvent gradient: 10min-10-95 Time (min.) 1 ) 0.0 0__________ 2) 1.00________ 3) 5.50_________ 4) 7.50_________ 5) 8.00_________ %B 10.0 10.0 95.0 95.0 1O0, M -S& p 000728 BEST COPY AVAILABLE Tuning Method Report Method: C :\MASSLYNX\AMELIA-RATS.PRO\ACQUDB\PFOS1-6KV Printed: Tue Oct 19 10:25:49 1999 Page 1 SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. Set Rdbk 1.60 40 5 0.2 150 250 1.59 -40 -5 153 248 Pressures Analyser Vacuum Gas Cell Rdbk 1.2e-4 4.6e-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set 15.0 15.0 2.0 0.0 4 650 Set Rdl 14.0 14.0 10 2.0 0.0 40 0 650 11 39 12 000729 Scannin Method K apert Method : C :\KMSLYMX\MCLXA*aiXTS.P*0\ACQUDS\10MIM-Pft>S-fOjUl-XS-PrOtA Laat Modified: Mon Oct 11 09:22:17 IKK Printed: Tue Oet 19 10:22:4 1999 Solvent Oelay I a i m ) : 0.00 Function : 1 MEM of 1 Maas Pair ( ESP- > Inter Channel Delay ( Secs ) : Span ( Daltons > : Stare Time { Mins ) : End Tine ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) Coll Energy <eV) Cone 1 413.00 169.00 0.30 30 IS Function SM of 1 Miao Fair ( ESP- Incer Channel Delay ( Seca ) : 0.03 Span ( Daltons ) : 0.00 Start Time ( Nina ) : 0.00 End Tiee I Mins > : 10.00 Repeats : 1 Channel Parent Daughter Dwell (Sees) Coll Energy (eV) Cone < V ) 1 499.00 99.00 0.30 45 CO F u n c tio n I of 1 maa Pair ( ESP- ) Inter Channel Delay < Secs > Span I Daltons ) : Start Tine ( Mins ) : End Time ( Mins ) : Repeats : Channel Parent Daughte 0.03 0 .0 0 0.00 10.00 1 Dwell (Secs) Coll Energy lev) Cone < V ) 1 427.00 90.00 0.30 40 Function : 4 M M of 1 Naas Pair ( BSP- > Inter Channel Delay ( Secs ) : Span ( Daltons ) : Start Time ( Mins l : End Time ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 l Dwell (Secs) Coll Energy (eV) Cone ( V 1 498.00 78.00 0.40 45 60 Masslynx Sample List Sam ple List: C :\M A S S LY N X \am elia-rats.P R O \S am pleD B \101999a.SP L Printed: Tu e Oct 19 14:10:27 1999 Page 1 P age Position: ( 1 . 1 ) File Name File Text MS File 1 101999001 MeOH 1 0 M IN -P F O S -P O A A -IS -P F O S A 2 101999002 MeOH 1 0 M IN -P F O S -P O A A -IS -P F O S A 3 101999003 Tox 145: R B L10139-H 2O blk-11, E xt S E E 10-13-99 10M IN -P FO S -P O A A -IS -P FO S A 4 101999004 Tox 145: RBL10139-Liver blk-11, Ext SEE 10-13-99 10M IN-PFO S-PO AA-IS-PFO SA 5 101999005 Tox 145: RBL10139-5 ppb-11. Ext S EE 10-13-99 10M IN -P FO S -P O A A -IS -P FO S A 6 101999006 Tox 145: RBL10139-10 ppb-11. Ext SEE 10-13-99 1 0 M IN -P F O S -P O A A -IS -P F O S A 7 101999007 Tox 145: RBL10139-25 ppb-11. Ext SEE 10-13-99 10M IN -P FO S -P O A A -IS -P FO S A 8 101999008 Tox 145: RBL10139-50 ppb-11. Ext S EE 10-13-99 1 0 M IN -P F O S -P O A A -IS -P F O S A 9 101999009 Tox 145: R B L10139-100 ppb-11. Ext S E E 10-13-99 10M IN -P FO S -P O A A -IS -P FO S A 10 101999010 Tox 145: RBL10139-250 ppb-11, Ext SEE 10-13-99 10M IN-PFO S-PO AA-IS-PFO SA 11 101999011 Tox 145: R BL1013 9 -5 0 0 ppb-11. Ext S E E 10-13-99 10M IN -P FO S -P O A A -1S -P FO SA 12 101999012 Tox 145: R BL10139-750 ppb-11, Ext S E E 10-13-99 10M IN -P FO S -P O A A -IS -P FO S A 13 101999013 Tox 145: RBL10139-1000 ppb-11. Ext SEE 10-13-99 10MIN-PFOS-POAA-IS-PFOSA 14 101999014 MeOH 10M IN -P FO S -P O A A -IS -P FO S A 15 101999015 Tox 1 4 5 :9R 03237M . D ay 4, Control. D:100 10M IN-PFOS-POAA-IS-PFOSA 16 101999016 Tox 145: 9R 03245M , D ay 1, 5 mg/kg, D :100 10M IN -P FO S -P O A A -IS -P FO S A 17 101999017 Tox 145: 9R 03246M , D ay 1. 5 mg/kg. D :100 1 0 M IN -P F O S -P O A A -IS -P F O S A 18 101999018 Tox 145: 9R 03247M , D ay 1, 5 mg/kg. D :100 1 0 M IN -P F O S -P O A A -IS -P F O S A 19 101999019 Tox 145: 9R 03248M , Day 1 ,5 mg/kg. D:100 1 0 M IN -P F O S -P O A A -IS -P F O S A 20 101999020 Tox 145: RBL10139-250 ppb-11-2. Ext SEE 10-13-99 10M IN-PFO S-PO AA-IS-PFO SA 21 101999021 M eO H 1 0 M IN -P F O S -P O A A -IS -P F O S A 22 101999022 Tox 145: 9R03249M , D ay 1 ,5 mg/kg, D:100 1 0 M IN -P F O S -P O A A -IS -P F O S A 23 101999023 Tox 145: 9R 03251M , D ay 4. 5 mg/kg, D:100 1 0 M IN -P F O S -P O A A -IS -P F O S A 24 101999024 Tox 145: 9R03252M , D ay 4, 5 mg/kg, D:100 1 0 M IN -P F O S -P O A A -IS -P F O S A 25 101999025 Tox 145: 9R 03253M , D ay 4. 5 mg/kg, D:100 1 0 M IN -P F O S -P O A A -IS -P F O S A 26 101999026 Tox 145: 9R03254M , D ay 4, 5 mg/kg, D:100 10M IN -P FO S -P O A A -IS -P FO S A 27 101999027 Tox 145: RBL10139-250 ppb-11-1. Ext SEE 10-13-99 10M1N-PFOS-POAA-IS-PFOSA 28 101999028 MeOH 10M IN -P FO S -P O A A -IS -P FO S A 29 101999029 Tox 145: RBL10139-H2O blk-11, Ext SEE 10-13-99 10MIN-PFOS-POAA-IS-PFOSA 30 101999030 Tox 145: RBL10139-Liver blk-11. Ext S E E 10-13-99 10M IN -P FO S -P O A A -IS -P FO S A 31 101999031 Tox 145: R B L10139-5 ppb-11. Ext S E E 10-13-99 1 0 M IN -P F O S -P O A A -IS -P F O S A 32 101999032 Tox 145: RBL10139-10 ppb-11. Ext SEE 10-13-99 33 101999033 Tox 145: RBL10139-25 ppb-11. Ext SEE 10-13-99 34 101999034 Tox 145: RBL10139-50 ppb-11. Ext SEE 10-13-99 10M IN -P FO S -P O A A -IS -P FO S A 10M IN -P FO S -P O A A -IS -P FO S A 10M IN-PFO S-PO AA-IS-PFO SA 35 101999035 Tox 145: RBL10139-100 ppb-11, Ext SEE 10-13-99 1MIN-PFOS-POAA-IS-PFOSA 36 101999036 Tox 145: R B L10139-250 ppb-11. E xt S E E 10-13-99 10M IN -P FO S -P O A A -IS -P FO S A 37 101999037 Tox 145: RBL101 3 9 -5 0 0 ppb-11, Ext S E E 10-13-99 10M IN -P FO S -P O A A -IS -P FO S A 38 101999038 Tox 145: RBL101 3 9 -7 5 0 ppb-11, E xt S E E 10-13-99 10M IN -P FO S -P O A A -IS -P FO S A 39 101999039 Tox 145: RBL10139-1000 ppb-11. Ext SEE 10-13-99 10MIN-PFOS-POAA-IS-PFOSA O00731 Masslynx - Sample List Sam ple List: C :\M A S S LY N X \am efla-rats.P R O \S am pleD B \101999a.S PL Printed: Tue Oct 1 9 1 4 :1 0 :2 7 1 9 9 9 page 2 P a a e P osition-(2 11 ^' Inlet File Bottle Inject V olum e Sam ple Type C one A Cone B C o n c C C o n c D C o n c E Cone F 1 10min-10-95 91 2 10min-10-95 91 3 10min-10-95 1 4 10min-10-95 2 5 10mm-10-95 3 6 10min-10-95 4 7 10min-10-95 5 8 10mln-10-95 6 9 10min-10-95 7 10 10min-10-95 8 11 10min-10-95 9 12 10min-10-95 10 13 10mirv10-95 11 14 10min-10-95 91 15 10min-10-95 12 16 10mln-10-95 13 17 10min-10-95 14 18 10min-10-95 15 19 10min-10-95 16 20 10mirv10-95 81 21 10min-10-95 92 22 10mirv10-95 17 23 10min-10-95 18 24 10mln-10-95 19 25 10min-10-95 20 26 10min-10-95 21 27 10min-10-95 82 28 10mirv-10-95 92 29 10min-10-95 1 30 10min-10-95 2 31 10min-10-95 3 32 10min-10-95 4 33 10min-10-95 5 34 10min-10-95 6 35 10mir>-10-95 7 36 10min-10-95 8 37 10min-10-95 9 38 10min-10-95 10 39 10min-10-95 11 10 10 -- 10 -- 10 -- - 10 -- 10 -- 10 -- 10 -- 10 ___ 10 -- 10 -- 10 ___ 10 -- 10 ___ 10 _ _ 10 10 -- 10 10 ___ 10 ___ 10 -- 10 ___ 10 -- 10 ___ 10 ___ 10 ___ 10 _ _ 10 ___ 10 _ 10 ___ 10 ___ 10 ___ 10 ___ 10 ___ 10 _ _ 10 10 10 __ _ _ 10 -- n----1 -- -- n ... ___ -- ___ -- ___ _ ___ ___ -- ___ ___ ___ -- _ ___ ___ _ ___ ___ ___ -- ___ ___ ___ ___ ___ ___ __ ___ ___ ,,,, ___ ___ ___ _ ... ...... _ ___ __ ___ _ ___ _ _ ___ ___ ___ _ _ _ __ _ ___ ___ -- ---- ___ . . . .., ___ _| , __ -T-- __ ___ - _ __ .._ _ __ ... _ ... ... ... u ___ ___ _ _ _ _ _ _ _ ___ __ .... _ ___ 1_ ,,. u r_ _ _ _ _ ___ _ .. . _ T__ _ _ ., _ _ _ _ _ 000732 FACT: DATA REVIEW SUMiMAJRYFORM *A Date: Data Analyst: FACT Study#: ~fcc - Hb/v Matrix/Timepoints: TaU uJ - liv e * /Leve. - e J - . A iM Data Review Sign-Off Analyst Review Name / Date: J a Technical Review Name / Date: Sample Lilt Set-up Analysis Date/Analyst /pzsrffc. **/f9 Ta-. Quality Assurance Review Name / Date:____________ Data Entry:. Instrument Amf'* Oz-fn Analyte: "PoAA Cdf^Q> Acceptable Linear Range: LQ;__ 3&~^j>h__ R-2: Q J U m Calibration Checks: AJa VAM S /M S D :__________ Data Status: Ml Extraction Blank: i LQ Matrix BUnk-J ^ / V ^ r - 4k+*.f Analyte: T fh $ CcHZ V,< Comments / Justifications: 0 7Zc /2 -3 > ^L f Mre. 4jut .ru-L. -Cte--d?.__"MziY__ tor^c -Irmi Tu 3 ~ ^ _ ,, k*J-----&* <- rtfe' / * ft K * UaJu*- oJ- Mcawe- 0 - 9f . Tfcte kJa.S d -ft*- h T / Oyo^ J i-h. - T a .^ / w A y / k s ______ Acceptable Linear Range: t2 > __________ Opis-h^ t > r T qA A L o . - 1 * 3 ^blt? LOQ: ) * 3> ytJ,_______ RA2: O . i l 'l / n z . Calibration Checks: H A Extracted Blank: }txlltu t. Q Matrix Blank: I f t S OQ T u l - t f / y i r jP`>tA^/ A x . g //h fegarJfp^-ettel fra*- 4l cu-rifc *> 4Uk 4 L Liytv&k lffJJ JU /<*SlUr~ 4L log. X- MS/MSD: Data Status: J A. Jill wAnalyte: i f e C tfi') Acceptable Linear Range: tA LO Q :___ ti ._____________ RA2:__ tik.________ Calibration Checks: AA MS/M SD:________ V A Data Satus: X))a Extracted Blank: /a Matrix Blank: A tK iA ___ L > h h i_ i l 1 . ` tZttjpL hfjjc* OcCclluudJefdJ__ //*A- o rrft ^_ 4t^ ___/9 >yoOtele. A, h u g ., franje torti- ta u re J > d diJ-ioe-*__ / L s Are*. Ce~uk~-t .PS h t c f /'sesie*J-. _fh~0BtC__k-J a. e*und'> ^'Vq. 3 ? iS A ^i fcjckS* oLi! J* I t yt a r i t i *f~_ "jrL& fifk- /s $*> bjC- ' ` t t 000733 FACT: DATA REVIEW SUMMARY FORM P^t 1 / 3. Date: Data Analyst: ?x* FACT Study It: 1oKft/t-Kfv Matrix/Timcpoints: 'EdlJ'b***fuy*, --cui. Sample List JozSflc Set-up Analysis Date/Analyst Instrument tofvsfrt fM ! nuha. oi 21ft PZjJ Analyte: Acceptable Linear Range: LOO: 3 = 7 R*2: O -ff s jp t- Calibration Checks: / / A MS/MSD:__ ______ t L Data Status: L Extraction Blank: Matrix Blank: le t* -U u *. 0 3 1 Data Review Sign-Off . Analyst Review Name/Date: jJAS , Technical Review . . . N am e/D ate: W tr +0 PuiiL llZ LkL 10 Quality Assurance Review N am e/D ate: Data Entry: A$ Oflb^ LAtC / m HI Comments / Justifications: 1U .3 c j P0^ k s * r ,e _ jbi 'H J- lft*M L- /e*sUT+~- '-h*, iodi. MtIamI y TjCc&A hXY*- -kisL --s** (2 X m &>Cia9c.T>a*J /^/frh - e s <S r ou> <g/*J - 7 d>er at <Lni*~-r~.. //)&? /olxr?J$9 000734 i ! ? e I I I 9 : 000735 SSSSSS3SC SsSsSSSSiSS s sss5ss;:I I SS25otiS5S I SSSS'g'SS ? &SSSig%g5Z 3 ~PfT^------ W / / y *Sp- $SSS2iSS32S2 otr I*' S t < * t r h c o o nr* H Ot H 0k -OHO mmmMhhmmm IIII111 s Ss : h rt o I IJ1 ; xsxs ft 3-3er4 e( *(el ei 4t l* -H 4 I K>l<M;o tj |s |s h ! 1? .. 3 i i M J Il !" J 3ljS ' jiiiil* > t 0t 0i 0kO01 9 OAAAOAKS 400MANSNSN INNNMfirtNN i\NNNNNNNS --- N N * ' ` ' " ,, _ , J, OS SO<. 52' s> a a &a a o o s J__A__n _n O_n.4 nooei oi Hft I S 0k I 0> Jk I A Jk i l NNNNNNNftNNN NNNNNNNI4NNN t* o o o o o o o o o o o w. M. M3u33Z3333. j 3j 3S5S22S322S222 OOMmmtfl i Ai niAIMAiAM } XXSrSl *SHHg P8 tS* 4S<SPSl *8H8p I/IOP OO O - 1 n * * ooooooooooooo 0AkA0kA0>A9>A0tA0>A0 kA0>A0kA0>A0A>0Ak MNNNNNNNNNNNN OOOOOOOOOOOOO 000736 i M jf 14 ? ! 3 3 NO 1 Quantify Compound l u n i i y Report TOX145-rabbit liver curva art. 10/22/* Mnr Banple U i t : C :\MABSLYMX\aeUa042 4. R 0 \ 0 n p l a M \ 1029 Last audified: Tuo Oct 2 09:34:39 1S9 Mathed: C :\MRMLYMC\aael laOC24 .PROXHathMX102599o Last Modified: TUO Oct 2 09:34:42 1999 Job Coda: Tinted: Tua Oct 2< 09:43:52 1999 Compound 3: 19 (Ch3) Ho m o 102599035 102599036 102599037 102599038 102599039 102599040 102599041 102599042 102599043 102599044 102599045 102599046 102599047 a^leliat Text MaOH Blank HaOH Blank TOX14S-RBL10229-K2O Blank-1, 10/22/99 RUM TOX145-RBL10229-Liver Blank-1, 10/22/99 RWM TOX145-RBL10229-Sppb-l. 10/22/99 RUN TOX145-RBL10229-12ppb-l, 10/22/99 RUN TOX145-RBL10229-30ppb-l, 10/22/99 RUN TOX145-RBL10229-60ppb-l, 10/22/99 RUN TQX14S-RBL1Q229-I20ppb-1, 10/22/99 RMM TOX145-RBL10229-3OOppb-l, 10/22/99 RUN TOX14S-RBL10229-6OOppb-l, 10/22/99 RNM TGK14S-RBLlQ229-900ppb-l, 10/22/99 RNM TOX145-RBll0229-1200ppb-i, 10/22/99 RNM Type Std Cone RT Standard Standard Standard Standard Standard Standard Standard Standard Standard 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 6.964 6.959 6.956 6.960 6.929 6.958 6.934 6.931 6.932 6.929 6.912 Area Cene. Plage tDev 3718 2208 2692 2725 2635 2559 2230 2409 2079 2041 2040 1.56 bb 0.93 bb 1.13 bb 1.15 bb 1.11 bb 1.08 bb 0.94 bb 1.01 bb 0.87 bb 0.86 bb 0.86 bb 56 -7 13 15 11 8 -6 1 -13 -14 -14 Pago 3 A oolia 042499: Q uantitated and p rin ted by iaa 10/24/99 0737  K II 0 B 1 P E i i 5 a ? E NMOs. 000738 > V W ~lWVI >)* J U * X i | M hh N W O* I JhtfMh Ol WWWMUAN> }A W* H H U f t *UN*WOOt**0 S5S5?ZSX5*iS5Si3S 3 BEST COPY AVAILABLE Q uantify C a lib ra tio n M pore fOX145- r a b b i t l l v a r o u r v o - o x t . 10/ 22/ 9 m m Compound 1 name: POAA (C hi) Coefficient o f Determination: 0.996986 * / P9 l 1 ; 000739 BEST COPY AVAILABLE Quantify Calibration apart TOXliS-rahbit llvar curve- ext. 10/22/tt ffl Compound 2 name: PFOS (Ch2) Coefficient o f Determination: 0.992922 Calibration curve: 6.34685 * x + 149.692 *" Pag 2 M anila M 2 I M ; Q u a n tita te d and p r in te d by ia a 1 0 /2 C /M BEST COPY AVAILABLE Quantify Calibration Moport ___ 1QK14S>rabbit l l v o r o u n o * o a t . 1 0 /3 2 /9 * MW Compound i name: IS (Ch3) Response Factor: 2378.96 Response type: External Std, Area jCurve type: RF 2.73e3-, ' Fapi 3 Response- 0 - L -----------------0 .0 0.1 I2 !? A aw lla 0S2499: guantitatod and p r in to d by i a a 1 0 /2 9 /9 9 --i------------ 1------------ 1------------ 1------------ :------------------------- Cone 0.4 0.5 0.6 0.7 0.8 0.9 1. OI 000741 BEST COPY AVAILABLE Q uantify C a lib ra tio n R eport TOX14S-rabbit liver curve- est. 10/22/9* W Compound 4 name: PFOSA (Ch4) 1 Coefficient o f Determination: 0.996087 Calibration curve: 17.5980 * x + 76.6733 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None ~~ Pag 4 000742 Hcnod Report Method file: Last Modified: Compound: Printed: C :\MASSLYNX\a m 11*062490.PRO\MethDB\102599c.mdb Tut Oct 28 09:34:42 1999C 1: POAA (Chi) Tue Oct 28 09:44:34 1999 Compound Na m : Internal Ref.: Quantify Trace: Cone, of Standards: User RF value: User Peak Factor: Integrate Window Factor: ChroMtogram m s s window: Peak Location Retention T i m (mins): Relative Retention T1m : RT Reference: Ti m Window {tins): Peak Selection: Response Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Concentration Units: Moise Peak-to-peak amplitude: Smooth Smoothing: Window size (scans): Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline Mximum: Peak Ssoaration Draw vertical threshold: Detect shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative area: Absolute area: PQAA (Chi) (Nona) TIC Cone. B 1.000000, Disabled 1.000000 2.000 1.00000s 6.889, Enabled 0.000, Disabled litonel 0.252 Nearest External Areas Linear Exclude 1/X None 91 Enabled 2 1 30.00 200.00 5.00 90.00 Disabled 30.00 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00. Disabled 000743 Method Report Method file : Last Modified: Compound: Printed: C: VHASS LYNX \amaiie062498.PRO\MethDB\l02599c.mdb Tue Oct 26 09:34:42 1999C 2: PFOS (Ch2) Tue Oct 26 09:44:34 1999 Compound Name: Internal Ref.: Quantify Trace: Cone, of Standard: User RF Value: User Peak Factor: Integrate Window Factor: Chromatogram mass window: Peak Location Retention Time (mins): Relative Retention Time: RT Reference: Time Window (mins): Peak Selection: Response Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Concentration Units: Noise Paak-lo-peak amplitude: Smooth Smoothing: Window size (scans): Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: Peak Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: Resoonse Threshold Relative height: Absolute height: Relative area: Absolute area: PFOS (Ch2) (None) TIC Cone, A 1.000000, Disabled 1.000000 2.000 1.00000a 7.109, Enabled 0.000, Disabled (None) 0.227 Nearest External Areas Linear Exclude 1/X None 96 Enabled 2 1 30.00 200.00 5.00 90.00 Disabled 30.00 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled Page 2 0007^4 Method Report Method file: Lest nodi fled: Compound: Printed: C:\MASSLYNX\ameUs062499.PRO\MethDB\102S99e.mdb Tu Oct 2 09:24:42 1999C 3: IS (Cti3> Tue Oct 24 09:44:34 1999 Compound Name: Internal Ref.: Quantify Trace: Cone, of Standards: User RF Value: User Peak Factor: Integrate Window rector: Chromatogram maas window: Peak Location Retention Time (minsi: Relative Retention Time: RT Reference: Time Window (mins): Peak Selection: ResDonse Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Concentration Units: Noise Peak-to-peak amplitude: Smooth Smoothing: Window aira (scans!: Number of smooths: Smooching stethod: Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: Peak Seoaration Draw vertical threshold: Detect shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative area: Absolute area: IS (Ch3) (Home) TIC rimed 1.000000, Disabled 1.000000 2.000 1.00000a 6.924, Enabled 0.000, Disabled (None! 0.252 Nearest External Areas Linear Exclude 1/X None 74 Enabled 2 1 30.00 200.00 5.00 90.00 Disabled 30.00 1.50, Dlaabled 0.00, Disabled 2.00, Disabled 0.00, Disabled Page 3 000745 Method Report Method file: Last modified: Compound: Printed: C: VMAS5LYWt\anelia062494.PAO\MethDB\l02S99c.mdb Tue Oct 26 09:34:42 1999C 4: PFOSA (Ch4) Tue Oct 26 09:44:34 1999 Compound Name: Internal Ref.: Quantify Trace: Cone, of Standards: User RF Value: User Peak Factor: Integrate Window Factor: Chromatogram mass window: Peak Location Retention Time (mins): Relative Retention Time: RT Reference: Time Window (mins): Peak Selection: Response Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: Fit Weighting: Axis Transfonaatloo: Concentration Units: Noise Peek-to-peek amplitude: Ssuaoth Smoothing: Window site (scans): Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: Peak Separation Draw vertical thrtshold: Detect shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative area: Absoluta araa: pf-o s a (Ch4) (Monel TIC Cone. B 1.000000, Disabled 1.000000 2.000 1.00000a 7.SI, enabled 0.000, Disabled (Monel 0.311 Nearest external Araas Linaar exclude 1/X None 319 enabled 2 1 30.00 200.00 5.00 90.00 Disabled 30.00 1.S0, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled Page 4 000746 AMELIA 062498: FACT Equipment Log *99114 Q uattro H, #6448E T** PAGE DATE: 10/25/99 ANALYST: ias STUDY NUMBER: T0145 MATRIX: Rabbit Liver DESCRIPTION: Curve FACT Method: ETS-8-7.0 Injection volume: lOuL Cycle time: 10 min. Electrode: Z-Spray Mobile Phase: (A)2.0 mM NH4CH3CQ2 (B )McOH TN-A- or stndrd number (A) 99085-11-3 (B) TN-A-2945 Prepared (date/by): (A) 10/21/99 sah (B) 10/20/99 ias Expires: (A) 04/00______________ (B) 04/00 Store at room temp? (YJ or N Other: G uard column: None__________________ Part number: na_________ Lot number: na Analytical column: Keystone Betasil____________________________________ Size: 2 x 50 mm________________ Type: C18___________ Sphere size: 5 um______ Part number: 055-701-2_____ Lot number: P9E11 Serial number:0591816Z Analytical parameters: Drying gas (L/hr): 300 ESI nebulizing gas (L/hr) 10 LC Flow rate: 300 uL/min. Back pressure: 62 bar Sheath gas (L/hr)J) HPLC solvent gradient: 10min-10-95 Time (min.) 1 ) 0. 0 0 ___________ 2) 1.00___________ 3) 5.50_________ 4) 7.50_____________ 5) 8.00_________ %B 10.0 10,0 95.0 95.0 10.0 000747 BEST COPY AVAILABLE Tuning Method Report Method: C : \MASSLYNX\AMELIA-RATS.PRO\ACQUDB\PROS1 - 6KV Printed: Mon Oct 25 1 0 :1 3 :5 6 1999 Rage 1 SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. Set Rdbk 1.60 40 5 0.2 150 250 1.60 -60 -6 151 250 Pressures Analyser Vacuum Gas Cell Rdbk 1.2e-4 4.5e-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set 15.0 15.0 2.0 0.0 4 650 Set Rdl 14.0 14.0 10 2.0 0.0 40 0 650 46 39 48 000748 Scanning Mathed Report Method: C:\MMLYXX\MCLXA-KAtS.faO\ACQUDS\lCMXM-PrOS~PafcA-XS-PVOSA Last Modified: Mon Oct U 01:22:17 I M S Printed: Mon Oct 25 10:13:20 1999 Solvent Delay ( mine ) : 0.00 function : 1 MRM of 1 Mass Pair ( ESP- ) Intar Channel Daley i[ Secs ) : Span ( Daltons } : Start Tine ( Mins ) : End Tine ( Mins > : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) Coll Energy (eV) Cone l 413.00 169.00 0.30 30 IS function : 2 M M of 1 Mass Pair ( ISP- ) Inter Channel Delay < Secs ) : Span ( Daltons ) : Start Tine ( Mins ) : End Tioe < Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) Coll Energy (eV) Cone ( V 1 499.00 99.00 0.30 45 60 function : 3 MSI of 1 M ji Pair ( ESP- > Inter Channel Delay ( Secs > : Span ( Daltons ) : Start Tine ( Mins ) : End Tine ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) Coll Energy (eV) Cone ( V 1 427.00 80.00 0.30 40 60 Function : 4 MHM of 1 Meee Pair ( ESP- > Inter Channel Delay <( Secs ) : Span ( Daltons ) : Start Tiae I Mins ) : End Tiae ( Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) Coll Energy (eV) Cone ( V 1 496.00 78.00 0.40 45 60 Pago 1 000749 Method Report Method Pile: Last Modified: Printed: c:\masslynx\amelia-rats.pro\acqudb\10min-10-95 Monday. October 25, 1999 10i1215 Monday, October 25, 1999 10)13:44 Page 1 BP1100 LC Pump Initial Conditions Solvents At B% Ct D% 90.0 10.0 0.0 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 0.300 10.0 0 400 30.0 30.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 5 entries which are : Time 0.00 1.00 5.50 7.50 8.00 At 90.0 90.0 5.0 5.0 90.0 B% 10.0 10.0 95.0 95.0 10.0 C* 0.0 0.0 0.0 0.0 0.0 Dt 0.0 0.0 0.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 Pressure 400 400 400 400 400 HP1100 LC Pump External Event Timetable The Timetable contains 3 entries which are : Time Initial 0.00 0.10 Column Switch Contact1 Off Off Off On Off Off Contact2 Off On Off Contact3 Off Off Off Contact4 Off On Off HP1100 Autosaapler Initial Conditions Draw Speed Eject Speed (il/min) Draw Position (mm) Stop Time (mins) Injection Volume(/il) Vial Number 200.0 200 0.00 9.00 10.0 13 000750 Masslynx Sample List Sam ple List: C :\M A S S LY N X \am elia-rats.P R O \S am pleD B \102599clSP L Printed: Mon Oct 2 5 10:13:12 1999 Page 1 Page Position: ( 1 .1 ) File Name File Text MS File Inlet File 1 102599035 M eO H Blank 10M IN-PFO S-PO AA-IS-PFO SA 10min-10-95 2 102599036 M eO H Blank 1O M IN -P F O S -P O A A -IS -P FO S A 10m in-10-95 3 102599037 TO X145-R B L10229-H 2O B la n k -1 ,10/22/99 RW W 10M IN-PFOS-POAA-IS-PFOSA 10min-10-95 4 102599038 TO X145-RBL10229-Liver B lan k-1,10/22/99 RW W 10M IN-PFOS-POAA-IS-PFOSA 10min-10-95 5 102599039 TOX145-RBL10229-5ppb-1,10 /22/99 RW W 10M IN-PFOS-POAA-IS-PFOSA 10min-10-95 6 102599040 TO X145-R B L10229-12ppb-1,10/22/99 RW W 10M IN-PFOS-POAA-IS-PFOSA 10min-10-95 7 102599041 TOX145-RBL10229-30ppb-1,10 /22/99 RW W 10M IN-PFOS-POAA-IS-PFOSA 10min-10-95 8 102599042 TOX145-RBL10229-60ppt>-1,10/22/99 RW W 10M IN-PFOS-POAA-IS-PFOSA 10min-10-95 9 102599043 TOX145-RBL10229-120ppt>-1,10/22/99 RW W 10M IN -PFO S-PO A A -IS-PFO SA 10min-10-95 10 102599044 TOX145-RBL10229-300ppb-1,10/22/99 RWW 1OMIN-PFOS-POAA-IS-PFOSA 10min-W -95 11 102599045 T O X 1 4 5 -R B L 1 0 2 2 9 -6 0 0 p p b -1 ,10/22/99 R W W 10M IN -PFO S-PO A A -IS-PFO SA 10min-10-95 12 102599046 TO X145-RBL10229-900ppb-1.1 0 /2 2 /9 9 RW W 10M IN -PFOS-POAA-IS-PFOSA 10min-10-95 13 102599047 TO X145-R B L10229-1200ppb-1,10/22/99 RW W 10M IN-PFO S-PO AA-IS-PFO SA 10min-10-95 000751 Masslynx Sample List Sample List: C :\M A S S LY N X \am elia-rats.P R O \S am pleD B \102599c.SP L Printed: Mon O ct 2 5 10:13:12 1999 Bottle Inject Volume 1 92 2 92 3 12 4 13 5 14 6 15 7 16 8 17 9 18 10 19 11 20 12 21 13 22 10 10 10 10 10 10 10 10 10 10 10 10 10 Page 2 P age Position: (2, 1) 000752 Date: Data Analyst: j2m _ FACT: DATA REVIEW SUM M ARY FORM Data ReviewSign-Off Analyst Review . Name / Date: 3 * S >aJz im p * - l 3. WCu lw r/T t FACT Study *: TrtMS. Matnx/Timepoints: "TZ'Ce*- Sample List: tornii Set-up Analysis Date/Analyst: rfufa m / m ., Technical Review Name / Date: g " 'o k f a I fa Quality Assurance Review N am e/D ate:_____________ Data Entry: 'Dm-NOT d e fcf-lp d OM. Instrument: S r y OZoffi Analyte; ~PoAA f t . i ' P Acceptable Linear Range: ' o j j L - "* / Z S 't j p L LOO: /.O0n> ExtractionBlank fjA RA2: 0, ff fS f_________ tJAMatrix Blank: F)K-Calibration Checks: -frai*. I3 `A * ~Yft> MS/MSD. Data Status: Gm i t i b M Analyte: f$t>6 ( c h i') Acceptable Linear Range: LOQ: J -O jy y i / < >^ r r ~ -* s'.* -. AJAExtracted Blank: SlC-Calibration Checks: Matrix Blank _ ^ 5 _ Trgfs Je. MS/MSD: Data Status: f f t fU fb T k d f-- Comments / Justifications: i d d i ----........ ffi_______________ f T jZ -tU ld i-... i>***-<' -Prf -A> u / tv ( f t Vto rti* * . i . ~fL /> L t t J f:tjL. O h x - ~^ a AA-- Ar ^ c , /to Uipt-ks -A ejd ro o d - k .a_ -kirL.-ff.-XbJV*,_-"%>* ''/zf/f* ^ TU y p p *J jHt+Js kx+e Jvo}fxJ ->~- -fL /*- QHtftr Jnuid*___ __ & >(/ fnu<AJtL. fi L i J / -/ jten J e O { A . f > o *^t. I * s i di**- -io*/ /- iowtv' f t j f / ftL .C*rue. J L r t tutve to. !idcAA 4 o A -J__ tJ < T ^ 4L. Analyte: ffirSA CcH-s^ Acceptable Linear Range: LOQ: r Extracted Blank A/M RA2: Matrix Blank / / 4 Calibration Checks: MS/MSD: DataSatus: s4. -iHsij-rt/n_______________________ ^ tt*. t v)jj>Lf Z'-asjj>L> .J fo.to JjJ* J > # j s J r o ^ v f eeccu^e- djfj h d dti/ief10'-? Jr dssL OX. of Hutv* 'cn-jyLs Litre -h o d o -c fo ______ o- v*-iScd<-i^(*Ju>~ &-d s b tJ d A c . y t - ~ e A VA.C t e t f ' - r i &)pr (v,Lr (w f bt (& (/ fa * ty& ,/ . Etot ^ spnemifaunUfafiJ. fm *r ar*M5 wm, occur af/cf UtfaM*** t f i u S A fltS - V M L- ^00753 Dale: Data Analyst 3* FACT: DATA REVIEW SUMMARY FORM Data Review Sign-OfT Analyst Review Name / Date: lef3- l^C u lo rh ^ fa c t study T gjc/yjr Matrix/Timepoints: - J *u. 0/& /l9 Technical Review Name/Date: Sample List Set-up Analysis Date/Analyst U ?Z49*. fa h th f Quality Assurance Review N am e/D ate: Data Entry: Comments / J u s t aitdionas:t ________________ 3s(jf) a r e a . C o t h r a k t j ________________ e u / L & > * * i s j c d A a u i c & -L*- Sa*ujle-i>. k>t>Clajo L a J Ore*. Aia -fi*, UiLcL d d * Lrd J -f*- A re a . ,omJ% Vs k - fL t - &Co*-<f d r o i j i e J C~J"Ac/ Js A L IlLfAtii CUS'IK'- ______ A V*iCoJce.(a.4i~a- U s & & ' dui 4-La TT a > * ____ i<** u*cAc, ? er ~4~ leu rs>ec'J S 1 jJ* HJ. /i j*c / e x h a . c c { s- hf a-r*J venere, sli-eJl tcr L* t**ec(*-- Jj. t*/*>/*9_________________________________ S\ A A H i r A U j O 0o > 4 I ** 1 I 3S"-rT?7SS 3 7 S7Sm3S73S 5S5S2S3S3S3SS 353 S53SSSSS J -3S3SSS3S55 ass ~3sssssa ! ll s i s silS I - S=SS2||S*S32 333 S"SS3333S SsSSss5333333 333 333333333 f-t-r'rr*f*'rrp.fr**r rrr* fr'^r-r-r'-r-r-r- S3S33SSSS 3 S S3S33SSSS S ""M SS* i ^ssssss i 88 l . nus!!!! g p?in?! llllll li Ili llillliii i l i 1 1 1illli iy - >00755 9S00u SsSsSSu.- s s s s s s s s s - 2 gggggggSg g g g'g'gggggss I sssSssssssrsSsHsSssSSsssSsSssi S ll5 l5 2 S 2 ls il5 Is il ls s is ? g g m m g m m m g g ? m m i S 3fi 5SSg?st:-e.B3s.sS^SsBasss.-..i S5gg5SS5S2SSSg5S5SaSS333t:S? t s SsI s SSu.m s ggggkkksb s k s s Hs s s ..h n sssskkksk SSS5SS5SSSSS5S55SS2SSSSSs m & g g g g g S S g g m m m g S g g g ie j! KKsSsasggs2sEssSoSssssg.oo.=8 bksskkkssssskkkkkskgksgkkgggg? .EK.SSgS S g .-Kggg f Quantity Compound M a n y import 10U 4 S - t M & 80 do* e o n f t m t ion- VOB/ri'OSAVfOAA at. 10/38/99 1 H u l l U a t : C: \MASSI.YW\soap030199 .proSSailaCMUOJI* u a e aodiflte: Pri Oct 07:02:9 199 Matted: C:\lOJMLnec\aoep0a0199.pro\teefem\102e b aodlflad: rri Oct 29 0:Sa:>5 1999 Job Ceda: 9rlatad: rri Oct 29 07:37:39 199 I ninnimi 4; zi (Ch4) MB* 1 102899001 2 102899002 3 102899003 4 102899004 S 102899005 C 102899006 7 102B99007 102899008 9 102899009 10 102899010 11 102899011 12 102899012 13 102899013 14 102899014 15 102899015 16 102899016 17 102899017 18 102899018 19 102899019 20 102899020 21 102899021 22 102899022 23 102899023 24 102899024 25 102899025 26 102899026 27 102899027 28 102899028 29 102899029 tarlai iat Toxt MaOS lit MaOB Bit POtix-99086-43-1. lppb- 9/10/99 M W FQLlx-99086-43-2. Sppb- 9/10/99 M W rOCix-99086-43-3, lOppb- 9/10/99 M W rOtix-99086-41-4, 25ppb- 9/10/99 M W rotix-99086-43-5. SOppb- 9/10/99 M W rCXix-99066-43-6. lOOppb- 9/10/99 M W ratc-99086-43-7, 250ppb- 9/10/99 M W ratix-990S6-43-l, SOOppb- 9/10/99 M W POlix-99086-43-9, 750ppb- 9/10/99 M W MaOB Ilk TOX145-Pros/PQAA la Twen-doaa-2ppb- 10/28/99 ZAS TOrU5-PPOS/POAA la TWan-m-4ppb- 10/28/99 ZAS fCMix-99086-43-4, 2Sppb- 9/10/99 M W NaOR Bit T0Xl45-pr0SA in Twaan-doaa^200ppb- 10/28/99 ZAS TOX145-PFOSA in Tvuan-aa-JOOppb- 10/28/99 ZAS POLbc-99086-43-7, 250ppb- 9/10/99 M W MaOB Blk PQLx-99086-43-1, lppb- 9/10/99 BMW raOx-99086-43-2. 5ppb- 9/10/99 M W rCMix-99086-43-3, lOppb- 9/10/99 BMW PCXi-X-99086-43-4. 2Sppb- 9/10/99 M W PCMix-99086-43-5. 50ppb- 9/10/99 BMW PCXix-99086-43-6. lOOppb- 9/10/99 BMW PCXix-99086-43-7. 2S0ppb- 9/10/99 BWW rOtix-99086-43-8. SOOppb- 9/10/99 BWW FCMiJC-99086-43-9. 750ppb- 9/10/99 BWW Typ Standard Standard Standard Standard Standard Standard Standard Standard Standard QC QC Standard Standard Standard Standard Standard Standard Standard Standard Standard Std cone 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 It* 7.081 7.0S3 7.102 7.101 7.103 7.109 7.102 7.105 7.120 7.124 7.134 7.130 7.134 7.138 7.124 7.127 7.145 7.143 7.125 7.151 7.141 7.147 7.149 7.145 7.121 Ara riapa 16 bb 4165 bb 4646 bd 4643 bb 4814 bb 4546 bb 4172 bb 2878 bd 2479 bb 2203 bb 3463 bb 3528 bb 3185 bb 3679 bb 3545 bb 2681 bb 3119 bb 3041 bb 2979 bb 2937 bb 2907 bb 2907 bb 2595 bb 2441 bb 2112 bb Oeae. BDav 0.00 -too 1.26 1.40 1.40 1.45 1.37 1.26 0.87 0.75 0.67 26 40 40 45 37 26 -13 -25 -33 1.05 1.07 0.96 5 7 -4 1.11 11 1.07 7 0.81 -19 0.94 0.92 0.90 0.89 0.88 0.88 0.78 0.74 0.64 -6 -8 -10 -11 -12 -12 -22 -26 -36 VtM 4 Bonp 020199: Q u a n tit t * a t e p r i t ad fey ia a a 1 0 /3 9 /9 9 j- L H----------------------------------------------------------------------------------------------------------------------------------------------------------------- * > / W / f r __________ Quantify CtliteMica tepore TCOUiS-twaaa o dos* oonirnatloo- m i / m u / N U ce. 1 0/at/t ina / i 000759 Quantify calibration -- port OQLWS-twnan 0 dosa oonfinaation- m i / r r o u / V Q U ant. 10/2/ ina -- ga 2 0007S0 Quantify Calibration aaporc TCK149>ewooa to dosa oaflrnatlon- pPOt/PfOSb/VOia axt. 10/21/19 laa *gm s 000761 Quantify Calibration noport *OX145>taaa 0 (ton ooaflcmatlOB- FfOI/rroil/IOU ont. 10/2/** Ina tag 4 000762 Method Report Method file: Last modified: Compound: Printed: C :\MASSLYMZ\soup020199.pro\MethDB\102899a.U> Fri Oct 29 06:53:35 1999 1: POAA (Chi) Fri Oct 29 07:11:25 1999 Compound Name: Internal Ref.: Quantify Trace: Cone, of Standards: User RF Value: User Peak Factor: Integrate window Factor: Chromatogram aaaa window: PQAA (Chi) (Nome] TIC Come. A 1.000000, Disabled 1.000000 2.000 l.OOOODa Retention Time (mins): Relative Retention Time: RT Reference: Time Window (mins) : Peak Selection: 7.152. Snabled 0.000, Disabled 0.35 Nearest Response Type: Response: beterne 1 Areas Polynomial Type: Point of Origin: Fit weighting: Axil Transformation: linear Exclude 1/X None Units: Peak-to-peak amplitude: 3 Smoothing: Window sire (scans): Number of smooths: Sa&othing method: Snabled 2 1 Join valley threshold: Reduce peak tailing: Raise baseline maximum: 30.00 200.00 S.00 Draw vertical thraahold: Detect shoulders: Shoulder threshold: 90.00 Disabled 30.00 Relative height: Absolute height: Relative area: Absolute area*. 1.50, Disabled 0.00. Disabled 2.00, Disabled 0.00, Disabled A+s-i'/nhl____J J f '/ Page 1 000763 Method Report Method file: Last modified: Compound: Printed: C :\MASSLYXX\aoup020199 .pro\MatbDB\102M9a.mdb Fri Oct 29 06:53:35 1999 2: FFOS (Ch2) Pri Oct 29 07:31:25 1999 Compound Name: Internal Ref.: Quantify Trace: Cone, of Staadarda: Uaer RP Value: Uaer Peak Paetor: Integrate Window Factor: Chromatogram mass window: PPOS (Ch2) [Nona) nc Cone. S 1.000000. Diaablad 1.000000 2.000 l.OOOODa Retention Time (mine): Relative Retention Time: RT Reference: Time Window (nine): Peak Selection: 7.335. Enabled 0.000. Disabled (None] 0.336 Nearest Reaponse Type: Response: External Areas Polynomial Type: Point of Origin: Pit Weighting: Axis Transformation: Linear Kccluda 1/X Mona Units: Peak-to-peak amplitude: sa Smoothing: Window sise (scans): Number of smooths: Smoothing method: Enabled 2 1 Join valley threshold: Reduce peak tailing: Raise caseline maximum: 30.00 200.00 5.00 Draw vertical threshold: Detect shoulders: Shoulder threshold: 90.00 Disabled 30.00 Relative height: Absolute height: Relative area: Absolute area: 1.50. Disabled 0.00. Disabled 2.00. Disabled 0.00, Disabled Page 2 000764 Method Report Method file: Last modified: Compound: Printed: C: \HASSLYNX\soup020199 .proUtethDSn02999a.mdb Fri Oct 29 06:53:35 1999 3: PPOSA (Ch3) Fri Oct 29 07:39:25 1999 Compound Nam: Internal Ref.: Quantify Trace: Cone, of Standards: Dear RF Value: User Peak Factor: Integrate Window Factor: Chromatogram mats window: PFOSA (Ch3) (Mona) TIC Cone. C 1.000000, Oiaablad 1.000000 2.000 1.OOOODa Retention T i m (mins): Relative Retention Tim: RT Reference: T i m Window (mins) : Peak Selection: 8.053, Enabled 0.000, Disabled [Monel 0.445 nearest Response Type: Response: fecternel Areas Polynomial Type: Point of Origin: Pit Weighting: Axis Transformation: Limar Exclude 1/X Hone Units: Peak-to-paak amplitude: 147 Smoothing: Window site (scans): Vuaber of smooths: Smoothing method: Enabled 2 1 Join valley threshold: Reduce peak tailing: Raise taseline maximum: 30.00 200.00 5.00 Draw vertical threshold: Detect shoulders: Shoulder threshold: 90.00 Disabled 30.00 Relative height: Absolute height: Relative area: Absolute area: 1.50. Disabled 0.00. Disabled 2.00. Disabled 0.00. Disabled . Page 3 000765 Method Report Method m e ; Lest modified: Compound: Printed: C:\MA5SLYtt\eoup020m.pro\MetfcDBU02B99a.mdb Fri OCC 29 0<:S3:3S 1999 4: IS (Chi) Pri Oct 29 07:39:29 1999 Compound Mens; Internel Ref.: Quantify Trace: Cone, of Standards: Oser rp Value: User Peak Factor: Integrate Window Factor: Chromatogram mass window: IS (Ch4) (Mona) TIC Fixed 1.000000, Disabled 1.000000 2.000 1.00000a Retention Time (mins): Relative Retention Time: RT Reference: Time Window (mins): Peak Selection: 7.190. enabled 0.000, Disabled (Monel 0.290 Dearest Response Type: Response: Bxtarnal Areas Polynomial Type: Point of Origin: pit Weighting: Axis Transformation: Linear Exclude 1/X one Units: Peak-to-peak amplitude: 70 Smoothing: Window size (scans): Number of smooths: Smoothing method: Snabled 2 1 Join valley threshold: Reduce peak tailing: Raise baseline maxisum: 30.00 200.00 5.00 Draw vertical threshold: Detect shoulders; Shoulder threshold: 90.00 Disabled 30.00 Relative height: Absolute height: Relative area*. Absolute area: 1.S0, Disabled 0.00. Disabled 2.00. Disabled 0.00, Disabled . 4 000766 Quattro II, #6414E SOUP 020199: FACT Equipment Log 99092 PAGE 1/1 DATE: 10-28-99 ANALYSTjas STUDY NUMBER: TOX145 MATRIX: Tween samples DESCRIPTION; dose confirmation FACT Method: Injection volume: 10 uL Cycle time: 10 min. Electrode: Z-Sprav______ MobUe Phase: (A)2,Q mM MH4CH3CQ2 (B) McQH------------------- TN-A- or stndrd number (A) 99085-11-3________ Prepared (date/by): 1A> 10/21/99 mmh_______ (B) TN-A-2S97(B) \Q/W 99 sah Expires: (A) 04/00______________ (B) 2Q1Q______ Store at room temp? @ or N Other:. G uard column: None__________________ Part number: na________ Lot number: na Analytical column:. Size..? x 59 t r n . Part number: 055-701-2 Type: _______ Lot number: P9EII Sphere size: 5 urn______ Serial number:0591804Z Analytical parameters: Drying gas (L/hri: 350 ESI nebulizing gas (L/hr) 13 LC Flow rate: 300 uL/min. Back pressure: bat Sheath gas (IVhr)Jl HPLC solvent gradient: 10min-10-95 Time (min.)____ U JLfifi__________ 2) JJ3Q_____ 3) _LSfi_______ 4 )_L5Q__________ 5 I M Q ___________ .%B-. 1M 1M _ 1Q. 2L. 1M . 000767 b e s t c o p y a v a il a b l e Tuning Method Report Method: C:\MASSLYNX\SOUP020199.PRO\ACQUDB\P7OS3 Printed: Thu Oct 26 15:21:34 1999 /y2&& Page 1 MS SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. MS Set Rdbk 1.60 60 5 0.2 150 250 1.59 -60 -7 153 249 Pressure* Analyser Vacuum Gas Cell Rdbk 6. le-5 4.le-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set Rdbk 14.0 14.0 0.9 0.0 4 650 3 Set Rdbk 14.0 14.0 60 2.0 0.0 40 0 650 28 38 28 000768 Method Report Method Filat Last Nodiiad: Printed! C l\M*SSLYMX\S009020199 .P*0\ACQDI\10min-10-95 Thursday, October 28, 1999 13i44>34 Thursday, Octobar 28, 1999 13i44i44 HP1100 LC f u b v Initial Conditions Solvents A% B% C% D% 90.0 10.0 0.0 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 0.300 10.0 0 400 30.0 30.0 HF1100 LC Fuav gradient Timetable The gradient Timetable contains 5 entries which are : Time A% B% C% D4 0.00 90.0 10.0 0.0 0.0 1.00 90.0 10.0 0.0 0.0 5.50 5.0 95.0 0.0 0.0 7.50 5.0 95.0 0.0 0.0 8.00 90.0 10.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 HP1100 LC Pump Internal Trent Timatable The Timetable contains 3 entries which are : Time Initial 0.00 0.10 Column Switch Contactl Off Off off on Off off Contact2 Off On Off Contact3 Off Off Off Contact4 Off on Off BP1100 jmtosampler Initial Conditions Draw Speed Eject Speed (pl/min) Draw Position (mm) Stop Time (mins) Injection Volume(pi) Vial Number 200.0 200 0.00 9.00 10.0 41 Page X Pressure 400 400 400 400 400 000769 Method* Ct\jaSSMaX\SOaP02019.PRO\RCQOBMUOMXM~PPO-POR*-prOR-XS U a t Modified: Iti Oct is 11:35:03 It# Printed: Thu Oct 21 13:44:1* 1# olvtat M a y ( a l u l i 0.00 Function : 1 m of l Musa pair ( MSP- ) Inter Channel Delay ( Secs ) t Spaa ( Daltons > a Start Tine ( Mina > : tnd Tine { Mins ) : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Sacs) Coll Energy (eV) Cone 1 413.00 14.00 0.30 30 15 Function : 2 M M of l Mass pair ( ESP- ) Inter Channel Delay <( Secs } : Span ( Daltons ) : Start Tine ( Mins ) : End Tins ( Mins } : Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) Coll Energy (eV) Cone 1 499.00 99.00 0.30 45 <0 Function a 3 M M of 1 Mesa pair ( ISP- ) Inter Channel Delay >1 Secs > a Span ( Daltons ) : Start Tine ( Mias ) i lad Tine ( Mias ) : Repeats a Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) Coll Energy (eV) Cone 1 498.00 78.00 0.30 45 SO Function t 4 MRM of 1 Mass pair ( SP- ) Inter Channel Delay i( Secs ) .* 0.03 Span ( Daltons ) : 0.00 Stare Tina ( Mina ) : 0.00 lad Tin ( Kins ) t 10.00 Rapests a 1 Channel Parent Daughter Dwell (Secs) Coll Energy (eV) Cone 1 427.00 80.00 0.30 40 60 000770 Masslynx - Sam ple List J Sam ple List: C :\M A S S LY N X \sou p020199.p ro \S am p leD B \102899a.S P L Printed: Thu Oct 2 8 13:44:09 1999 f /* s/9 9 /n ta r page 1 P age Position-(1 1) File Nam e File Text MS File 1 102899001 M eO H Blk 2 102899002 M eO H Blk 10M IN-PFO S-PO AA PFOSA-IS 10M IN-PFO S-PO AA PFOSA-IS 3 102899003 FCM ix-99086-43-1, 1ppb- 9/10/99 RW W 10M IN -P FO S -P O A A - PFOSA-IS 4 102899004 FCMix-99086-43-2, 5ppb- 9/10/99 R W W 10M IN -P FO S -P O A A - PFOSA-IS 5 102899005 FCM ix-99086-43-3,10ppb- 9/10/99 RW W 6 102899006 FCMix-99086-43-4, 25ppb- 9/10/99 RW W 10 M IN -P FO S -P O A A ' PFOSA-IS 10M IN-PFOS-POAA- PFOSA-IS 7 102899007 FCMix-99086-43-5, 50ppb- 9/10/99 R W W 10M IN-PFO S-PO AA- PFOSA-IS 8 102899008 FCMix-99086-43-6,100ppt>- 9/10/99 RW W 10MIN-PFOS-POAA- PFOSA-IS 9 102899009 FCMix-99086-43-7, 250ppb- 9/10/99 R W W 10M IN-PFOS-POAA- PFOSA-IS 10 102899010 F C M ix-99086-43-8, 500pp b- 9 /1 0 /9 9 R W W 10M IN -P F O S -P O A A - P FO S A -IS 11 102899011 F C M ix-99086-43-9, 750pp b- 9 /1 0 /9 9 R W W 10M IN-PFO S-PO AA- PFOSA-IS 12 102899012 M oO H Blk 10M IN-PFO S-PO AA- PFOSA-IS 13 102899013 T O X 14 5 -P F O S /P O A A In T w e e n -d o s e -2 p p b -10 /28/9 9 IAS 10M IN -P F O S -P O A A - P FO S A -IS 14 102899014 TO X145-P FO S/P O A A in Tw een -m s-4p pb -10/28/99 IAS 10M IN -PFO S-PO A A - PFO SA-IS 15 102899015 FCMix-99086-43-4, 25ppb- 9/10/99 R W W 1OMIN-PFOS-POAA- PFOSA-IS 16 102899016 M e O H Blk 1OMIN-PFOS-POAA- PFOSA-IS 17 102899017 T O X 1 4 5 -P F O S A in T w e e n -d o s e -2 0 0 p p b -10 /28/9 9 IAS 1OMIN-PFOS-POAA- PFOSA-IS 18 102899018 T O X 1 4 5 -P F O S A in T w e e n -m s -3 0 0 p p b -10 /28/9 9 IAS 1OMIN-PFOS-POAA- PFOSA-IS 19 102899019 FCM ix-99086-43-7,250ppb- 9/10/99 R W W 1OMIN-PFOS-POAA- PFOSA-IS 20 102899020 M eO H Blk 1OMIN-PFOS-POAA- PFOSA-IS 21 102899021 F C M ix-99086-43-1, 1ppb- 9 /1 0 /9 9 R W W 10M IN -P F O S -P O A A - P FO S A -IS 22 102899022 FCM ix-99086-43-2, 5ppb- 9/10/99 R W W 10M IN-PFO S-PO AA- PFOSA-IS 23 102899023 FCM ix-99086-43-3,10ppb- 9/10/99 R W W 10M IN-PFO S-PO AA- PFOSA-IS 24 102899024 FCMix-99086-43-4, 25ppb- 9/10/99 R W W 10M IN-PFO S-PO AA- PFOSA-IS 25 102899025 FCMix-99086-43-5, 50ppb- 9/10/99 RW W 10MIN-PFOS-POAA- PFOSA-IS 26 102899026 FCM ix-99086-43-6,100ppb- 9/10/99 RW W 10M IN-PFO S-PO AA- PFOSA-IS 27 102899027 FCM ix-99086-43-7,250ppb- 9/10/99 RW W 10MIN-PFOS-POAA- PFOSA-IS 28 102899028 FCMix-99086-43-8, 500ppb- 9/10/99 RW W 10MIN-PFOS-POAA- PFOSA-IS 29 102899029 FCMix-99086-43-9. 750ppb- 9/10/99 RW W 10M IN-PFO S-PO AA- PFOSA-IS 000771 M asslynx - Sam ple List Sam ple List: C:\M ASSLYN X\soup020199.pro\S am pleD B \102899a.SP L Printed: Thu Oct 28 13:44:09 1999 Inlet File B ottle Inject V olum e S am ple Type C one A C o n c B C o n cC 1 10m in-10-95 91 2 10m in-10-95 91 3 10min-10-95 1 4 10min-10-95 2 S 10min-10-95 3 6 10min-10-95 4 7 10min-10-95 5 8 10min-10-95 6 9 10min-10-95 7 10 10min-10-95 8 11 10m in-10-95 9 12 10mirt-10-95 92 13 10min-10-95 10 14 10min-10-95- 11 15 10min-10-95 4 16 10min-10-95 92 17 10min-10-95 12 18 10min-10-95 13 19 10min-10-95 7 20 10m in-10-95 92 21 10m in-10-95 1 22 10min-10-95 2 23 10min-10-95 3 24 10min-10-95 4 25 10min-10-95 5 26 10min-10-95 6 27 10min-10-95 7 28 10min-10-95 8 29 10min-10-95 9 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 ~ 10 -- 10 -- 10 -- 10 -- ------ ------ -- -- ---- -- ------ ------ ------ ------ ---- -- ---- -- ------ ------ ------ -- -- -- ---- -- ------ ------ ------ -- ---- ------ -- --: -- ------ ------ ------ ------ ------ ------ ------ ------ /a , Page 2 Page Position: ( 2. 1) ^00772 JL FACT: DATA REVIEW SUMMARY FORM Data ReviewSign-OfT Analyst Review Nim e / Dele: ,. ''U t/H Matnx/Timepoints: Td-lnnv -- (d*Jrff SAmple Lift itOSffA. Set-up Analysis Date/Analyst: Instrument 3** "/oehy U fa OLz</n fo-v9~ c / Aaetvte: T o A A ( c m 'fi Acceptable Linear Range: i/-3oyyl T/^^te4- LOQ: f.3j>pL Extraction Blank: f t s s [/& |R A2 --AZIU , Matrix Blank: /**S 4L*. U a Calibration Checks: 04- - t* J e Ir ti* - ' ,a> /o Data Status: hASf ( U f t A t l , .... Analyte: 7fcS C C H z-'f ~ 'P ilth g u r t . "3**O lk h i Acceptable Linear Range. f c - S o j j b ____________ LOQ: l ? - - 3 ^ L _______ Extracted Blank: b s s '/i* ~ lo Q RA2: b.fgzHi Calibration Checks: Matrix Blank: Q vta Jcs 'M o* iOQ Bu-oe. /y a* - -/3~A MS/MSD:.3 2 % ,j S ^ Data Status: fa wAnalyte: _ S u - r C a t s ') Acceptable Linear Range: A/A L Q - ____________ 2!_____ *"*________&__ Calibration Checks: A/A MS.MSD: NffiT________ DataSarur. Extracted Blank: fJ * Matrix Blank: tJ A j,} f/M jkjin l l f f k g Quality Assurance Review Name / Date:_____________ DataEntry:. V m G ^ U Rammenta/Justificadons: d e l* } ^ *^ C c u J n u . ! . ( ns^ L f t z ^ y ^ i j tert mJ- Z< LjLv -A a^v. * l L - fitrivaefta*- 4 l * * l c , - ^ a k M'rgfy/ujec / yCu X C*.n*c 4*____ lisp ia fil^ . loda. rv.* p ~$aI x t y / W Stomfie<uditj aJ&Jecih h.ckj>yroiL uJ /e tu A e r f <JU .CW&iyL, '***U n. ____h u e d J O , i U t s U.*4 iL s poinj- -excfu JeJIn 'f i x CkJfu<. ~(i J t3 ^U e J iltj A- roe yje- 4 4 a l~ %nt L*_*. &4Hjca*JL gj&dcj. L U i 'vou.*cf( C U t L y l l i t Qj^Ufle. - K s 'ik i tfpL Ctirutpu< ds j^'H7ZIU* ' l < x dal fp j w i J t & I t tier U t over *J b 1` ITmii 7proT>rh(a lt -Jo ~U- JaJo- ~ J*S G a / i f j a v e cl o t u ^ f i if O.H C dref S a p L s g * J 4 L . ms ft**b Imve Lui. ~~J&s *i'thf___________ _ 000773 FACT: DATA REVIEW SUMMARY FORM Date: Data Analyst: "lash 'M S FACT Study*: 1 Matrix/Timepoints: Zed-Ltkr ~-fonJr*lj JoS*- A* * l * - e J * f t l t * Sample Use Set-up Analysis Date/Analyst t e n * .__________________ /. ZXa s " / s f c l Instrument A u .J i+ - Q Z ' f f S Data ReviewSign-OfT Analyst Review Name / Date: , __________ Technical Review Name / Date: A tatr i-a JkJlhh Quality Assurance Review Name / Date:_____________ Data Entry: it, -tr J*. p a y - 1 _______ iM d lln s l^ C o m m e n ts/Ju ttM ca tio n s:____________________________ ^ Lon) ledjx>i*ds i tZ-3Z Jjfb hjcrc *-oJ- knhv -llaj. 4le luc r e e t c l u e r / - A ' a * . ~ J Cittftn. > 0 ( 6 6L Hj*f* 000774 000775 6 6 / t / t t * * * -TO U O O pu *o p &Aa 'i*A T T W -S M X O * ssSSSSKS;;;::;:;;;:::;;: IliSSIIIIlliIi!II I s s s s s s s '- ~ ,, ,, i c c ssssj =" " p p || p ||H ="~' ?? es SSSasssE. ggggg SSSSSsse. gggggg SssSSSSssSS 2SSSSSsSS 35S53S 2S5S55515Ss s slsssis ss ssssss IsssS silssssilss t 5 "So0ooo Soo ooooo SoooSS S - K o o o o o SSKgggggg g g g g g g ^g ig gg SS9 gggggg ggggS gggggg gggggg SSSSggggg ggggggfggg f ? 3 M' ' u -o is li I i. S i, ^ S- i. i :l Sg S| Sg g f V* I r s ! ps i l *1 a i S O O O \ U) ssSsisSsSsSsssisHsssisassiSssHsSsasScssss ssssisssssssssssssfissassB ssS sssssssassss ! S H S * K , O O o S S S o S S S E o O o S o O o 5 o 5 5 2 S S o 0 0 0 0 of ssssisgggiiiigiiibbsggsgggssgsssisiigggggg!' a3 M ! 1 r - T -- f?5S8SS?;s5 1S1S "27 S'? r>si>HHOOviAgin i fe SSSSSSSSSSSSSSSSSS SB8 2S gssssssssss SPSSSSSSSSS8SSSSSS SSSSSS PSS SPEP322SSSS O O H O ** O O O O O O O O O O O O O r-t -*o o >-o o o -* -* >- - ^ -* <-*o o i 5 != s5 f= i! s is ii sii m m m i SsssssIslsIslSIS issisi HI s iili:!!!-! 000777 i -i* 1 1 1 3 3 I r e c i I ! i ? s 8 0 0 m m im m m u m m m m m m m m m l p f Sssss. ggggSSSSE SsEsssss. ggggggggs SS533`sSSSS333SsS3aS2332g3Sa33sS'sa22a'*a llis S s s S S S ^ S S S ^ IS S lH S s ls s S ls s lIlls lS H S S s a s S l SgE5s~oooSo2|g5oooo-N.SSoSlsSK2K.,,,,H SSSiggSgSSaSSSSgii.SSggSScigESSSSgKS ii||iiig??Sf?iiii|gi3 U ? I ------------------------------------------- !----------------------------------------- Quantify Calibration Import TOX145-rat livor, Day99 dos* and control- cat. 11/4/99 IWW Compound 1 name: POAA (Chi) Coefficient of Determination: 0.989198 Calibration curve: 0.973462 * x + 119.913 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None ~~ PmJ* 1 000779 Quantify Calibration Report TOX145-rat livar, Day29 dean and control- oat. 11/4/99 MVW Compound 2 name: PFOS (Ch2) Coefficient o f Determination: 0.982749 Calibration curve: 9.51640 * x + 260.801 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None Rage 2 AMlia 062499 : Quantitated and raviowed by las on 11/9/99 n0780 Quantify Calibration import ___ TOX145-rat livor, Day29 do and control- oxt. 11/4/99 KRW Compound 3 name: Surr (Ch3) Response Factor: 4773.57 Response type: External Std, Area Curve type: RF t Pag 3 ~ 000781 Quantify Calibration Hepert T0X14S-rat livar, Day29 doao and control- axt. 11/4/99 W W Compound 4 name: PFOSA (Ch4) Coefficient o f Determination: 0.989845 C alibration curve: 17.2655 * x + 131.101 iResponse type: External Std, Area jCurve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None Pi q o 4 ~~ 000782 Method Report Method fil#: Last modified: Compound: Printed: F:\amelia backup *p99Sua*li*-r*ta.pro\M*ChDB\110599a.Jadb Mon Nov 0 08:20:27 1999C 1: POAA (Chi) Mon Nov 08 08:56:36 1999 Coapound Name: Internal Ref.: Quantify Traca: Cone, of Standards: User RF Value: User Peak Factor: Integrate Window Factor: Chromatogram mass window: Peak Location Retention Time tains): Relative Retention Time: RT Reference: Time Window (mins): Peak Selection: Response Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Concentration Units: Noise Peak-to-peak amplitude: Smooth Smoothing: Window size (scans): Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: Peak Separation Draw vartical threshold: Detect shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative area: Absolute area: POAA (0)1) (None! TIC Cone. A 1.000000, Disabled 1.000000 2.000 1.00000a 6.97, Enabled 0.000, Disabled [None] 0.278 Neerest external Areas Linear Exclude 1/X None 530 enabled 2 1 30.00 200.00 5.00 90.00 Disabled 30.00 1.S0, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled Page 1 000783 Method Report Method file: Lest Modified: Compound: Printed: F:\amelia backup sep99\amelia-rats.pro\MethDB\110S99m.mdb Mon Mov 0 06:20:27 1999C 2: PFOS (Ch2) Mon Nov 08 08:58:38 1999 Compound Name: Internal Ref.: Quantify Trace: Cone, of Standards: User RF Value: User Peak Factor: Integrate Window Factor: Chromatogram mass window: Peak Location Retention Tine (mins): Relative Retention Time: RT Reference: Time Window (mins): Peak Selection: Response Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Concentration Units: Noise Peak-to-peak amplitude: Smooth Smoothing: Window size (scans): Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: Peak Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative area: Absolute area: PFOS (Ch2) [None] TIC Cone. B 1.000000, Disabled 1.000000 2.000 l.OOOODa 7.149, Enabled 0.000, Disabled (None] 0.299 Nearest External Areas Linear Exclude 1/X None 56 Enabled 2 1 30.00 200.00 5.00 90.00 Disabled 30.00 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled Page 2 000784 Method Report Method file: Lest modified: Compound: Printed: F:\emelie backup sep99\amelia-*rats.pro\MethI>B\I10599a.pdb Mon Mov 0 08:20:27 1999C 3: Surr (Ch3) Mon Nov 0 08:56:38 1999 Compound Name: Internal Ref.: Quantify Trace: Cone, of Standards: User RF Value: User Peak Factor: Integrate Window Factor: Chromatogram mass window: Peak Location Retention Time (mina): Relativa Retention Time: RT Refarenca: Time Mindow (mina): Peale Selection: Responso Responso Type: Responso: Calibration Curvos Polynomial Typo: Point of Origin: Fit Weighting: Axis Transformation: Concentration Units: Worse Peak-to-peak amplitude: Smooth Smoothing: Window size (scans): Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: Peak Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative area: Absolute area: Surr (Ch3) (None] TIC Fixed 1.000000, Disabled 1.000000 2.000 1.0000DS 7.023, Enabled 0.000, Disabled [None] 0.310 Nearest External Areas Linear Exclude 1/X None 80 Enabled 2 1 30.00 200.00 5.00 90.00 Disabled 30.00 1.50, Disabled 0.00, Disabled 2.00. Disabled 0.00, Disabled Peg 3 000785 Method Report Method file: Last modified: Compound: Printed: F:\amelia backup sep99\amelia-rata.pro\NethDB\110S99a.4sdb Mon Nov 08 00:20:27 1999G 4: PFOSA (Ch4) Mon Nov 08 08:50:36 1.999 Compound Name: Internal Ref.: Quantify Trace: Cone, of Standards: User RF Value: User Peak Factor: Integrate Window Factor: Chromatogram mass window: Peak Location Retention Time (mins): Relative Retention Time: RT Reference: Time Window (mins): Peak Selection: Response Response Type: Response: Calibration Curves Polynomial Type: Point of Origin: Fit Weighting: Axis Transformation: Concentration Units: Noise Peak-to-peek amplitude: Smooth Smoothing: Window size (scans): Number of smooths: Smoothing method: Baselines Join valley threshold: Reduce peak tailing: Raise baseline maximum: Peak Separation Draw vertical threshold: Detect shoulders: Shoulder threshold: Response Threshold Relative height: Absolute height: Relative area: Absolute area: PFOSA <Ch4) (None] TIC Cone. C 1.000000, Disabled 1.000000 2.000 l.OOOODa 7.770, Enabled 0.000, Disabled (None] 0.200 Nearest External Artaa Linear Exclude 1/X None 02 Enabled 2 1 30.00 200.00 5.00 90.00 Disabled 30.00 1.50, Disabled 0.00, Disabled 2.00, Disabled 0.00, Disabled Page 4 000786 AM ELIA 062498: FACT Equipm ent Log 99114 Q uattro II, #6448E & PA G E _______ DATE: 11/05/99 ANALYST: ias STUDY NUMBER: TOX145 MATRIX: rat liver DESCRIPTION: Day 29 control and dose FACT Method: ETS-8-7.0 Injection volume: 10 uL Cycle time: 10 min. Electrode: Z-Spray Mobile Phase: (A)2.0 mM NH4CH3CQ2 (B )McOH TN-A- or stndrd number (A) 99085-11-6______ (B) TN-A-2997 Prepared (date/by): (A) 10/30/99 sah________ (B) 10/29/99 mee Expires. (A) 04/00_______________ (B) 04/00 Store at room temp? [Y] or N Other: G uard column: None__________________ Part number: na Lot number: na Analytical column: Keystone Bctasil____________________________________ Size: 2 x 50 mm________________ Type: C18___________ Sphere size: 5 um_____ Part number. 055-701-2 ___ Lot number: P9E11 Serial number.089815 S Analytical parameters: Drying gas (L/hr): 300 ESI nebulizing gas (L/hr) 10 LC Flow rate: 300 uL/min. Back pressure: 62 bar Sheath gas (L/hr)_0 HPLC solvent gradient: 10min-10-95 Time (min.) 1) 0.00___________ 2 ) 1.00____________ 3 ) 5.50__ 4) 7.50____________ 5) 8.00____________ %B 10.0 10.0 95.0 95.0 10.0 A A 0787 BEST COPY AVAILABLE Tuning Method Report Method: C :\MASSLYNX\AMELIA062498.PRO\ACQUDB\PFOSl-6KV Printed: Fri Nov 05 09:43:09 1999 Page 1 MS SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. Set Rdbk 1.60 40 5 0.2 150 250 1.60 -40 -3 151 253 Pressures Analyser Vacuum Gas Cell Rdbk 1.2e-4 4.8e-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set Rdbk 15.0 15.0 2.0 0.0 4 650 11 Set Rdbk 14.0 14.0 10 2.0 0.0 40 0 650 12 40 10 000788 Scanning Mathod ftaport Mathod: C: \MhflSLY>0(\AMBLlAO<249a.VnO\ACaUDSMQKlN>PfOS-MAA-ZS-nrOSX Loat Hodified: Mon Oct U 07:22:1? 1999 Printed: Fri Nov 05 09:26:14 1999 Solvent Delay ( ina ) : 0.00 Function : 1 MUM of 1 Hass Fair { ESP- ) Inter Channel Delay i. Secs ) : Span Daltons : Start Tiae : M m s End Tine < Mins Repeats : Channel Parent Daughter 0.03 0.00 0.00 10.00 1 Dwell (Secs) coll Energy (eV) Cone < v 1 413.20 169.00 0.30 30 15 Function : 2 MRM of 1 Maas Fair ( ESP- > Inter Channel lela, Span Ca.'.ms Star: Time M m s End T.e . M m s Repeats : Channel Parent Secs ) : Daughter 0.03 0.00 0.00 10.00 1 Dwell (Sees) Coll Energy (eV) Cone 1 V 1 499.30 99.00 0.30 45 60 e l i %* 0 Function : 3 MM Fair { ESP- ) Inter Channel Delay [ Secs ) : Span Daltons Start Time Mm s End ?:ae M m s Repeats : Cttar.r.c* ri:rv. Daughter 0.03 0.00 0.00 10.00 1 Dwell (S e c s) Coll Energy (eV) Cone ( V 1 4 " .. ; 90.00 0.30 40 60 Function : 4 M M of 1 Meaa Fair ( ISF- ) Inter Channel Dela/ i Seca > : 0.03 Span ' Daltons 1 0.00 Start Time ' Mini 0.00 End Time < Mins ) : 10.00 Repeats : 1 Channel Pare-.-. Daughter IVell (Secs) Coll Energy (eV} Cone ( V ) 78.00 0.40 45 60 sago 1 000789 Method Report Method File: Last Modified: Printed: C :\MASSLYNX\AHELIA062498.PRO\ACQDB\10min-10-95 Friday, November 05, 1999 06 22124 Friday, November 05, 1999 0926>28 Page 1 HP1100 LC Pump Initial Conditions Solvents A% B% C% D% 90.0 10.0 0.0 0.0 Flow (ml/mm) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature LeftCC) Oven Temperature RightCC) 0.300 10.0 0 400 30.0 30.0 HP1100 LC Pump Gradient Timetable The gradient Timetable contains 5 entries which are : Time 0.00 1.00 5.50 7.50 8.00 A% 90.0 90.0 5.0 5.0 90.0 B% 10.0 10.0 95.0 95.0 10.0 C% 0.0 0.0 0.0 0.0 0.0 D% 0.0 0.0 0.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 Press 400 400 400 400 400 HP1100 LC Pump External Event Timetable The Timetable contains 3 entries which are Time Initial 0.00 0.10 Column Switch Contactl Off Off Off On Off Off Contact2 Off On Off Contact3 Off Off Off Contact4 Off On Off HP1100 Autosampler Initial Conditions Draw Speed Eject Speed (ji1/min) Draw Position (mm) Stop Time (mins) Injection Volume(jil) Vial Number 200.0 200 0.00 9.00 10.0 32 000790 Masslynx - Sam ple List Sample List: C :\M A S S LY N X \am ella062498.P R O \S am pleD B \11059a.SPL Printed: Fri Nov 05 09:25:34 1999 ige i Page Positior : ) File Name File Text MS File 1 110599001 M eO H Blank 10M IN -P F O S -P O A A -IS -P F O S A 2 110599002 MeOH Blank 10M IN -P F O S -P O A A -IS -P F O S A 3 110599003 MeOH Blank 10M IN -P F O S -P O A A -IS -P F O S A 4 110599004 TOX145-RBL11049-W BIk-1, RW W - Box 99-211 10 M IN -P F O S -P O A A -IS -P F O S A 5 110599005 TO X145-RBL11049-RBL Blk-1, RW W - Box 99-211 1O M IN -P F O S -P O A A -IS -P FO S A 6 110599006 T O X 145 -R B L 11049-6ppb-1, R W W -B o x 99-211 10M IN -P F O S -P O A A -IS -P F O S A 7 110599007 TOX145-RBL11049-12ppb-1, RW W - Box 99-211 10 M IN -P F O S -P O A A -IS -P F O S A 8 110599008 TOX145-RBL11049-30ppb-1, RW W - Box 99-211 10 M IN -P F O S -P O A A -IS -P F O S A 9 110599009 TOX145-RBL11049-60ppb-1, RW W - Box 99-211 1 0 M IN -P F O S -P O A A -IS -P F O S A 10 110599010 TO X145-R B L11049-120ppb-1, R W W - Box 99-211 10 M IN -P F O S -P O A A -IS -P F O S A 11 110599011 TO X145-R B L11049-300ppb-1, R W W - Box 99-211 10M IN -P F O S -P O A A -IS -P F O S A 12 110599012 TO X 1 45-R B L 11049-600ppb-1, R W W - Box 99-211 1 0 M IN -P F O S -P O A A -IS -P F O S A 13 110599013 TO X 1 45-R B L 11049-900ppb-1. R W W - Box 99-211 10M IN-PFO S-PO AA-IS-PFO SA 14 110599014 TOX145-RBL11049-1200ppt>-1, RW W - Box 99-211 10M IN-PFO S-PO AA-IS-PFO SA 15 110599015 MeOH Blank 10M IN -P F O S -P O A A -IS -P F O S A 16 110599016 TO X145-R B L, 9R 03240-300ppb-M S, 11/4/99- Box 99-211 1O M IN -P F O S -P O A A -IS -P FO S A 17 110599017 TO X145-R B L, 9R 03240-300ppb-M SD , 11/4/99 Box 99-211 10M IN -P F O S -P O A A -IS -P F O S A 18 110599018 TOX145-RBL, 9R03240/M/Day29/Control, 11/4/99 10M IN -P F O S -P O A A -IS -P F O S A 19 110599019 TO X145-RBL, 9R03241/M/Day29/Control, 11/4/99 10 M IN -P F O S -P O A A -IS -P F O S A 20 110599020 TOX145-RBL, 9R03242/M/Day29/Control, 11/4/99 10 M IN -P F O S -P O A A -IS -P F O S A 21 110599021 TO X145-R B L11049-300ppb-C C 1 -1, R W W - Box 99-211 1 0 M IN -P F O S -P O A A -IS -P F O S A 22 110599022 MeOH Blank 10 M IN -P F O S -P O A A -IS -P F O S A 23 110599023 TOX145-RBL, 9R03243/M/Day29/Control, 11/4/99 10M IN -P F O S -P O A A -IS -P F O S A 24 110599024 TOX145-RBL, 9R03244/M/Day29/Control, 11/4/99 10 M IN -P F O S -P O A A -IS -P F O S A 25 110599025 TOX145-RBL. 9R03255/M/Day29/5mg/kg, 11/4/99 10 M IN -P F O S -P O A A -IS -P F O S A 26 110599026 TOX145-RBL, 9R03256/M/Day29/5mg/kg, 11/4/99 10 M IN -P F O S -P O A A -IS -P F O S A 27 110599027 TO X145-RBL, 9R03257/M/Day29/5mg/kg, 11/4/99 10 M IN -P F O S -P O A A -IS -P F O S A 28 110599028 TOX145-RBL11049-300ppb-CC1-2, RW W - Box 99-211 10M IN -P F O S -P O A A -IS -P F O S A 29 110599029 MeOH Blank 1 0 M IN -P F O S -P O A A -IS -P F O S A 30 110599030 TOX145-RBL, 9R03258/M/Day29/5mg/kg, 11/4/99 10M IN -P F O S -P O A A -IS -P F O S A 31 110599031 T O X 1 45-RBL, 9R03259/M /Day29/5m g/kg, 11/4/99 1 0 M IN -P F O S -P O A A -IS -P F O S A 32 1105S9032 TOX145-RBL11049-300ppb-CC1-1, RW W - Box 99-211 10M IN -P F O S -P O A A -IS -P F O S A 33 110599033 M eO H Blank 10M IN -P F O S -P O A A -IS -P F O S A 34 110599034 TOX145-RBL11049-W BIk-1, RW W- Box 99-211 10M IN-PFO S-PO AA-IS-PFO SA 35 110599035 TO X145-RBL11049-RBL Blk-1. R W W - Box 99-211 10M IN -P F O S -P O A A -IS -P F O S A 36 110599036 TO X145-RBL11049-6ppb-1, RW W - Box 99-211 1 0 M IN -P F O S -P O A A -IS -P F O S A 37 110599037 TOX145-RBL11049-12ppb-1, RW W -Box 99-211 1 0 M IN -P F O S -P O A A -IS -P F O S A 38 110599038 TO X 145 -R B L 11049-30ppb-1, R W W - Box 99-211 10M IN -P F O S -P O A A -IS -P F O S A 39 110599039 TOX145-RBL11049-60ppb-1, RW W - Box 99-211 10M IN -P F O S -P O A A -IS -P F O S A 40 110599040 TO X145-RBL11049-120ppb-1, RW W - Box 99-211 1 0 M IN -P F O S -P O A A -IS -P F O S A 41 110599041 TO X145-R B L11049-300ppb-1, R W W - Box 99-211 10M IN -P F O S -P O A A -IS -P F O S A 42 110599042 TO X145-RBL11049-600ppb-1, RW W - Box 99-211 1 0 M IN -P F O S -P O A A -IS -P F O S A 43 110599043 TOX145-RBL11049-900ppb-1, R W W -B ox 99-211 1 0 M IN -P F O S -P O A A -IS -P F O S A 44 110599044 TO X145-RBL11049-1200ppb-1. RW W - Box 99-211 1 0 M IN -P F O S -P O A A -IS -P F O S A "n0 7 9l Masslynx - Sample List Sam ple List: C :\M A S S L Y N X \am elia0 624 98.P R O \S am p le D B \1 105 99a .S P L Printed: Fri Nov 0 5 09:25:34 1999 Page 2 P aae Position- (2 11 y Inlet File Bottle Inject Volume Sample Type C o n e A C o n e B C o n e C C o n e D C o n e E C o n e F 1 10m in-10-95 91 2 10min-10-95 91 3 10min-10-95 91 4 10min-10-95 1 5 10min-10-95 2 6 10min-10-95 3 7 10mm-10-95 4 8 10mm-10-95 5 9 10min-10-95 6 10 10min-10-95 7 11 10m in-10-95 8 12 10min-10-95 9 13 10min-10-95 10 14 10min-10-95 11 15 10min-10-95 92 16 10min-10-95 12 17 10m in-10-95 13 18 10min-10-95 14 19 10min-10-95 15 20 10min-10-95 16 21 10min-10-95 24 22 10min-10-95 92 23 10min-10-95 17 24 10min-10-95 18 25 10min-10-95 19 26 10min-10-95 20 27 10m in-10-95 21 28 10min-10-95 25 29 10min-10-95 93 30 10min-10-95 22 31 10m in-10-95 23 32 10min-10-95 24 33 10min-10-95 93 34 10min-10-95 1 35 10min-10-95 2 36 10min-10-95 3 37 10min-10-95 4 38 10min-10-95 5 39 10min-10-95 6 40 10min-10-95 7 41 10mm -10-95 8 42 10min-10-95 9 43 10mm-10-95 10 44 10m in-10-95 11 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 00073Z FACT: DATA REVIEW SUM M ARY FO RM Date: f/n /i11 Data Analyst. FACT Study *: JjUL. Matnx/Timepoints: L l u . 9 JaSe. Ji/k a u x - C e l " /l/ft Simpla List- Set-up Analysis Date/Analyst Instrument JU M L L ---------------------------------------------------t S " /h /1i 2 - Anahrte: ?OAA {? uac t) Acceptable Linear Range: /Z3ppL T J imtffL LOQ:. L Extraction Blank le ss J Ia k ft? R*2: 0 -V O tS L Matrix Blank Jean ILa k Od Calibration Cheeks: K- JC L MS/MSP: Dftlft moi 11SeA' C, Tftry.f DaU Status: j n l j ' ______ LA_Ct_ _ LL Analyte: 7f S CfitKC Z, ^t<3> Acceptable Linear Range: tZ-$oj>j>b LOQ: /i-3*>sjmj>> LL R*2: /). 99/9Z 7 Extracted Blanfkc l/e ss U ma QQ Matrix Blank OtreJr J it - Lo Calibration Checks: OK -/? * / MS/MSD:___ A)0l- Q n o . \ ^ ____|A) l ^ Data Status: m. Erksd ( A l, u lirh s T F o S A C T iulC 3*) Acceptable Linear Range: i, - /3 r o b ALOQ:. Extracted Blank le s s R-2: Q . f m f i . Matrix Blank le ss 'Ji-K CO Calibration Cheeks: f) k - n i * ____________________ MS.MSD: D^-a ho}- U.. A f P/ritriti rom__ g n f l l t f DataSatus: 0 * I l l b s K 1! LAC, H115 / 9 Data Review Sign-OfT Analyst Review Name / Date: 3 * * *J*hi Technical Review Name / Date:`S n o f r * .. / h Jpv- K - ^ Quality Assurance Review Name / Date:___________ Data Entry.. IC IS i l Commenti / Justifications: --IrUJ M IWtrhj -C4/3 ^ A- P&fpb.j -- fort i t e / V h j j L t JJ& h -- A lt. A ie lte o lltH . U am J ____ As* p*uds-Jticre. (Tjtclu/f,/ ~tfry*a* 4 u C * u * . J J / S ^ u a . / . ltj A J d t- K iy 4LoJ IKj A 4 /t4iHnihf-ltteetLA-tLlu O&cU A iajkroeumnA I/t(LUeJss AJ jJUlJZa/utLl - Ths "lu, Z ^ log/Ctcvue PoikJ . I/^pdL. kstLS______ IiduAclas f l MS n j A>db*. Jl**3>t CCHteC rtauirenuil A He._________ M l CUM* &XK *l&Atipici Qwr a .oAty raw efpwnteJc Jo- JL JJh - 1 Cifinnmtld- D(]) ' POAfi y tfl fl/tf <k -fetA4fJ~etuttJPl-c /> kt*e d*d<J S - r ^ l o i_______ kjvs___N*VWS - f l i /* T j - U 2' 000793 FACT: DATA REVIEW SUMMARY FORM Data Analyst: FACT Study : l "T o i / / S ' ____________________________________ Matnx/Timepoints: f b y J o te J r U /iM - < / " / j i f f Sunpl*Lilt H/Offt*______________________________ Set-up Analyst Dite/Analyst Instrument JL "`A t . ji^L W~ Analyte: ^ t y r ( f f C * / ) Acceptable Linear Range: A l o q ________ ___________ HAR"2: __________ Extraction Blank: M atrix Blank: A/fl Calibratioa Checks: JtifL. MS/MSD: o i k 4 a r f f i - Q n c J ^ l t - J a l a r>c4 Data Statu:_________ _________________ ______________________ 1* Silirl'Wl Data Review Sign-Off Analyst Review Name / Date: Jks nf<>94 Technical Review N am e/ Dale: g | r fro p a y . lt>Y 1 (AC I | / k / <? Quality A ssurance Review N a m e/D a te :___________________________ _____________ _ D ata R a tty :_______ L h O I l l i r i c i ___________________ Comments/ Justifications: _ _ *fJ J&eA **** AJO yfee J i/ u J ta H S h ~Mj -_____ J ifiJ in . f t d o v ' /h* *t* *J'. - J * S f 'k t J _____________ `'/h / i r 2^Z- 000794 & i s l s 8 O O O v l CO in Print! j O M XI^O'P ' ^ < 0 U O r* iscaS ssc. s ggssssst: s lrS ksssss in ; SscsSssc. SSSSSSSSE 5 8 sssssksshsb ,, 3SsSSSSEss b g&m gg}{g& ? ssiBscoooo ; esssssssss s ,, sissll S |S S S " S3S s**m m *s i sSsSo,,oo ssssssassss s ? o* o~ <K o 3 i iS I ^ a------- 5 5'"'7377"'? jggggsssgspasssgssssasgggsssagsa taaasa a s s s a s s s i s s a s s s a h s s s s s s p 3 3 g S 3 3 ^ ; y s H a S 3 3 S 3 !i;g ss-ss-si-saS sas^ I Sgggggggg 28 " ^ 3 2 S III g ssssggggg i "325i lilfliii h httCCbf <i0b<0 m I ? | 3 ?s|i?s lass isti m 1! lila 1! ssaaassssssaaasasasassas 000796 i I 3 s 7" 7" 7 saggssssssssgsggggggsgggssasgssss 2 ^ g ^ 3 3 5 ^ i 3 s " d s a g s ^ ssgsss is s s s s s ii; i- s 8 3 s q j - )c S ssIsssS sS sssissssss^ asssggggg *3S3S g sgggggggg i *3S2S o S <y O a slsss aaaaa C O i T TS S 5 53 ? a 't a I 000797 i I o I & f t tG d O O i3t:S5StiSSKt:" SSSSS:5ECCPS ! 4) JoV a tagjA- n a ^ daW r\*\ iW 5S5SS iiii ? ggggggggg ggggggggg lIIIilgSSgSSI^SSSSSSgSSSSgSSK s i s 3lslllsllls.===!==t=3llllisl=l5 ssisissszssnsessssssszsssss?? s SSS3Cg2SSg3SSSSg5gggSSSSSS ,,,,.P^-SgSSSSSSgiiiiiiu.iiii ? ? Quantity Calibration Baport TQXl4S>rat livar day 9 doaa dilations* out. 11/4/99 m w t '>00799 Q U A tlfy C a lib ra tio n M p o rt T O X 1 4 5 -ra t l l v a r , d a y 2 * d o a a d i l u t i o a a - a x t . 1 1 /4 /9 9 ***** * tm o* 2 0 0 S 0 0 aQ u a n t i f y C a l i b r a t i o n l a p o n ____ *O X14S>rat liv o r , da y d o a o d i l u t i o n s - a n . 1 1 / 4 / 9 9 *** * ,*** 3 080l Q u a n tify C a lib ra tio n R aport ____ T O X liS -ra t U n r , day 2 dosa d ilu tio n s - o u t. 1 1 /4 /tf W * an* 4 OOOBOZ Method Report Method file: beat modified: Compound: Printed: C:\MASSLYjnc\aeup020199.pro\MethDSU11099e.mdb Thu Mov 11 07:OS:22 1999 1: POAA (fuse 1) Thu Mov 11 07:34:44 1999 Confound Naae: Internal Ref.: Quantify Trace: Cone, of Standarda: Uaer HP Value: Uaer Peak factor: Integrate Window factor: Chromatogram naae window: POAA (Pune 1) (None] TIC Caoc. A 1.000000, Oieabled 1.000000 2.000 1.00000a Retention Tine (nine): Relative Retention Time: RT Reference: Time Window (mine) : Peak Selection: 7.047, enabled 0.000, Diaabled [Mona} 0.24 beareat Reaponae Type: Reaponae: External Arena Polynomial Type: Point of Origin.* fit Weighting: Axis Transformation: Linear Rxrlude 1/X Mone Unite: Peak-to-peak amplitude: S2 Smoothing: Window aise (scans): Number of amootha: Smoothing method: tnabled 2 1 Join valley threehold: Reduce peak tailing: Raiae baaeline maximum: 30.00 200.00 5.00 Draw vertical threahold: Detect ahouldere: Shoulder threahold: 90.00 Diaabled 30.00 Relative height: Absolute height: Relative area: Abeolute area: 1.50, Diaabled 0.00, Diaabled 2.00, Diaabled 0.00, Diaabled 1P e g * 000S03 .. t.jj ' - Method Report Method file: Last modified: Compound: Printed: C:\MASSLyKX\soup020199. pro\MethDB\111099a.adb Thu MOV 11 07:01:22 1999 2: PROS (Pune 2) Tfcu Nov 11 07:14:44 1999 Coapouad Nene: Internal Ref.: Quantify Trace: Cone, of Standards: User RP Value; User Peak Factor: Integrate Window factor: Chromatogram Maas window: pros (Pune 2) (Nona) TIC Cone. S 1.000000, Disabled 1.000000 2.000 l.OOOODa Retention Tine (nina): Relative Retention Tie RT Reference: Tine Window (Mins) : Peek Selection: 7.284, Enabled 0.000. Disabled [Monel 0.279 Mearest Response Type: Response : External Areas Polynomial Type: Point of Origin: Pit weighting: Axis Transformation: Linear Exclude l/X Bone Units: Feak-co-peak amplitude: 98 Smoothing: Window sise (scans): Number of smooths: Smoothing method: Enabled 2 1 Join valley threshold: Reduce peek tailing: Raise baseline maximum: 30.00 200.00 5.00 Draw vertical threshold: Detect shoulders: Shoulder threshold: 90.00 Disabled 30.00 Relative height: Absolute height: Relative erse: Absolute arse: 1.50, Disabled 0.00, Disabled 2.00. Disabled 0.00. Disabled Page 2 000804 Method Report Method file: last modified: Compound: Printed: C: \KASSLYNX\soup020199-pre\NeehDE\111099e.mdb m i Rov 11 07:09:22 1999 4: Surr (Func 4} Thu Mov 11 07.-J4.-44 1999 Compound Heme: laeemel Ref.: Quantify Trace: Cone, of Standards: User RF Value: User Peak Factor: Integrate Window Factor: Chromatogram mass window: Surr (Func 4) [None] TIC Fixed 1.000000. Disabled 1.000000 2.000 1.00000s Retention Tine (ados): Relative Retention Tims: RT Reference: Time Window (nine): Peak Selection: 7.141. enabled 0.000. Disabled [None] 0.27 Nearest Reaponae Type: Response; External Areas Folynoadal Type: Point of Origin: Fie Weighting: Axis Transtarnation: linear Exclude 1/X one Units: Peak*to-peak amplitude: 92 Smoothing: Window site (scans): Number of smnnths: Smoothing aurttood: Enabled 2 1 Join valley threshold: Reduce peak tailing: Raise beaeline maximum: 30.00 200.00 5.00 Draw vertical threshold: Detect shoulders: Shoulder threshold: 90.00 Disabled 30.00 Ralstive hsight: Absolute height: Relative ares: Absolute ares: 1.50. Disabled 0.00. Disabled 2.00. Disabled 0.00, Disabled Fege 4 000805 Q uattro II, #6414E J*9 "fbht SOUP 020199: FACT Equipment Log 99092 PAGE 1/1 DATE: 11-10-99 ANALYSTS STUDY NUMBER:TOX 145 MATRIX: rat liver DESCRIPTION: dilutions-dav29 FACT Method: ETS-8-7.0 Injection volume: 10 uL Cycle time: 10 min. Electrode: Z-Sorav______ Mobile Phase: (A12.0 mM NH4CH3CQ2 TN-A- or stndrd number (A) 99085-11-21 (B)_MsQH-------------------- (B) T.tLA-338.6----------- Prepared (date/by): (A ) 11/6/99 sah________ (B) 1V W 9 -- Expires: (A) 04/00______________ (B) 2Q1Q____________ Store at room temp? @ or N Other: _____________________ G uard column: None__________________ Part number: na Lot number: na_______________________ Analytical column: Keystone Betasil----------------------------------------------------- Size: 2 x 50 mm________________ Type:_lS___________ Sphere sizc:.5 um------------------- Part number: 055-701-2_________ Lot number: P9E11 Serial number:05918Q4Z_______ Analytical parameters: Drying gas (L/hr): 350 ESI nebulizing gas (L/hr) 13 LC Flow rate: 300 u&min. Back pressure.,^., bar Sheath gas (L/hr)_Q __ HPLC solvent gradient: 10min-10-95 TimstminJ------- l)s m _______ 2LLQQ_________ 3 ) 5.50 4) ZSQ______ 5IMQ_______ 3EL iM 1M _ MS S IS . m o. 000806 tJEST COPY AVAILABLE. Tuning Mathod Report Method: C:\MRSSLYNX\SO0PO2OX99.PRO\ACQDDB\PFOS3 Printed: Wed Nov 10 10:49:41 1999 Page 1 MS SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. MS2 Set Rdbk 1.60 40 5 0.2 150 250 1.61 -60 -6 150 250 Pressures Analyser Vacuum Gas Cell Rdbk 6.0e-5 4.le-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set Rdbk 14.0 14.0 0.9 0.0 4 650 3 Set Rdbk 14.0 14.0 10 2.0 0.0 40 0 650 37 38 40 000807 Method Report Method Pila: last Modilad: Printadi C! \KXSSLYKXVSOUP020199.PRO\ACQUDB\10nin-lQ-95 Wednesday, November 10, 1999 10i43t07 Wednesday, November 10, 1999 10i49i20 HP1100 1C Puas> Initial Conditions Solvents A% B% C% D% 90.0 10.0 0.0 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 0.300 10.0 0 400 30.0 30.0 HP1100 1C Puro Gradient Timetable The gradient Timetable contains 5 entries which are : Time 0.00 1.00 5.50 7.50 8.00 A% 90.0 90.0 5.0 5.0 90.0 B% 10.0 10.0 95.0 95.0 10.0 c% 0.0 0.0 0.0 0.0 0.0 D% 0.0 0.0 0.0 0.0 0.0 Plow 0.300 0.300 0.300 0.300 0.300 BPiioo ic Puro External Event Timetable The Timetable contains 3 entries which are : Time Initial 0.00 0.10 Column Switch Contactl Off Off Off On Off Off Contact2 Off On Off Contact3 Off Off Off Contact4 Off On Off HP1100 Autosarolar Initial Conditions Draw Speed Eject Speed (ul/min) Draw Position (mm) Stop Time (mins) Injection Volume(ul) Vial Number 200.0 200 0.00 9.00 10.0 91 Paga 1 Pressure 400 400 400 400 400 000808 Masslynx - Sample Lit Sample Ust: C:\MASSLYNX\soup020199.proVSampleDB\111099a.SPL Printed: W ed Nov 10 10:48:56 1999 Page 1 P age Position: ( 1 , 1 ) File Nam e File Text MS R ie 1 111099001 M eO H Blank 10M IN -P FO S -P O A A -P FO S A -IS 2 111099002 MeOH Blank 10M IN -P FO S -P O A A -P FO S A -IS 3 111099003 MeOH Blank 10M IN -P FO S -P O A A -P FO S A -IS 4 111099004 TOX145-RBL11049-W BIk-2, RW W 10M IN -P F O S -P O A A -P F O S A -IS 5 111099005 TOX145-RBL11049-RBLBIk-2, RW W 10M IN -P F O S -P O A A -P F O S A -IS 6 111099006 TO X145-R B L11049-6ppb-2, RW W 10M IN -P F O S -P O A A -P F O S A -IS 7 111099007 TO X145-RBL11049-12ppb-2, RW W 10M IN -P FO S -P O A A -P FO S A -IS 8 111099008 TO X145-R B L11049-30ppb-2, R W W 10M IN -P F O S -P O A A -P F O S A -IS 9 111099009 TO X145-R B L11049-60ppb-2, R W W 10M IN -P F O S -P O A A -P F O S A -IS 10 111099010 TO X145-RBL11049-120ppb-2, RW W 10M IN -P FO S -P O A A -P FO S A -IS 11 111099011 TO X 1 45-R B L 11049-300ppb-2, R W W 10M IN -P F O S -P O A A -P F O S A -IS 12 111099012 TOX145-RBL11049-600ppb-2, RW W 10M IN -P F O S -P O A A -P F O S A -IS 13 111099013 TO X145-RBL11049-900ppb-2, R W W 10M IN -P F O S -P O A A -P F O S A -IS 14 11 1099014 T O X 145 -R B L 11049-1200ppb-2, R W W 10M IN -P F O S -P O A A -P F O S A -IS 15 111099015 M eO H Blank 10M IN -P F O S -P O A A -P F O S A -IS 16 111099016 TO X145-RTL, 9R03255/M /Day29/5m g/kg-D100,11/4/99 10MIN-PFOS-POAA-PFOSA-IS 17 111099017 TO X 1 45-R T L , 9R 03 256 /M /D ay 29/5 m g /kg -D 100 ,11/4/99 10M IN -P FO S -P O A A -P FO S A -IS 18 111099018 T O X 1 45-R T L , 9R 03 257 /M /D ay 29/5 m g /kg -D 100 ,11/4/99 10M IN -P FO S -P O A A -P FO S A -IS 19 111099019 TO X145-RTL, 9R 03258/M /D ay29/5m g/kg-D 100,11/4/99 10MIN-PFOS-POAA-PFOSA-IS 20 111099020 TO X145-RTL, 9R 03259/M /Day29/5m g/kg-D100,11/4/99 10MIN-PFOS-POAA-PFOSA-IS 21 111099021 T O X 1 45-R B L 11049-300ppb-CC 1 -2, R W W 10M IN -P FO S -P O A A -P FO S A -IS 22 111099022 MeOH Blank 10M IN-PFOS-POAA-PFOSA-IS 23 111099023 TO X145-RBL11049-W BIk-2, RW W 10M IN -P FO S -P O A A -P FO S A -IS 24 111099024 TOX145-RBL11049-RBLBIk-2, RW W 10M IN -P FO S -P O A A -P FO S A -IS 25 111099025 TO X145-RBL11049-6ppb-2, RW W 10M IN-PFOS-POAA-PFOSA-IS 26 111099026 T O X 1 45-R B L 11049-12ppt>-2, R W W 10M IN-PFOS-POAA-PFOSA-IS 27 111099027 TO X145-RBL11049-30ppb-2, RW W 10M IN -P FO S -P O A A -P FO S A -IS 28 111099028 TOX145-RBL11049-60ppb-2, RW W 10M IN -P FO S -P O A A -P FO S A -IS 29 111099029 TO X145-RBL11049-120ppb-2, RW W 10M IN -P FO S -P O A A -P FO S A -IS 30 111099030 T O X 1 4 5 -R B L 1 1049-300ppb-2, R W W 1 0 M IN -P F O S -P O A A -P F O S A -IS 31 111099031 TO X145-R B L11049-600ppt>-2, R W W 10M IN -P F O S -P O A A -P F O S A -IS 32 111099032 TOX145-RBL11049-900ppb-2, RW W 10M IN -P FO S -P O A A -P FO S A -IS 33 111099033 TO X145-RBL11049-1200ppb-2, RW W 10M IN-PFOS-POAA-PFOSA-IS 34 111099034 TO X145-RBL11049-900ppb-2, RW W 10M IN-PFOS-POAA-PFOSA-IS Maulynx Sample Liat Sample Ust: C:\M ASSLYNX\soup020199.pro\Sam pleDB\111099a.SPL Printed: W e d Nov 10 10:48:56 1999 Inlet File Bottle Inject Volum e Sam ple Type Cone A C o n c B C o n c C 1 10m in-10-95 91 2 10m in-10-95 91 3 10m in-10-95 91 4 10min-10-95 1 5 10min-10-95 2 6 10min-10-95 3 7 10min-10-95 4 8 10min-10-95 5 9 10min-10-95 6 10 10min-10-95 7 11 10m in-10-95 8 12 10min-10-95 9 13 10min-10-95 10 14 10m in-10-95 11 15 10min-10-95 92 16 10min-10-95 12 17 10min-10-95 13 18 10min-10-95 14 19 10min-10-95 15 20 10min-10-95 16 21 10m in-10-95 17 22 10min-10-95 92 23 10min-10-95 1 24 10min-10-95 2 25 10min-10-95 3 26 10min-10-95 4 27 10min-10-95 5 28 10min-10-95 6 29 10min-10-95 7 30 10min-10-95 8 31 10m in-10-95 9 32 10min-10-95 10 33 10m in-10-95 11 34 10min-10-95 12 10 ... 10 10 10 -- 10 -- 10 -- 10 -- 10 --10 -- 10 -- 10 -- 10 10 -- 10 -- 10 -- 10 10 10 10 -- 10 -- 10 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 _ 10 10 -- ... ... ---- -- ... -- ---- -- -- ---- -- ---- -- -- ... -- ------ -- ------ -- ---- -- ... ---- -- ... ---- -- ... -- ---- -- ... -- ... -- -- ... -- ... -- -- -- ... -- . . . . . . __ ... ... ... -- -- ---- -- . . . __ -- ... -- . . . __ __ . . . ... ... -- -- Page 2 P age Position: ( 2 , 1 ) 000810