Document 1QJeGrVrXzw7vOeaXqY5gNDvK

3M G en eral O ffices 3M Cemer S). Paul. MN 55144-1000 651 733 1110 September 24, 20Q3t By Hand Delivery Document Processing Center (7407) Office of Pollution, Prevention and Toxics U.S. Environmental Protection Agency 1200 Pennsylvania Avenue, N. W. Washington, DC 20460 Attention: Section 8(e) Coordinator Re. TSCA Section 8(e) Submissions Dear Sir/Madam: 3M Company ("3M") requests that EPA place the attached studies in the TSCA Section 8(e) docket. We have included a master index for these studies identifying the study title, test substance and CAS number. A Confidential Business Information (CBI) version of this index and the studies also is being submitted today pursuant to EPA procedures. 3M has not provided CBI substantiation with this submission, but would be willing to do so at the Agency's request. 3M has concluded that data in these studies may not be, strictly speaking, "corroborative" of previously reported or published information as defined in EPA's reporting guidance or otherwise potentially may warrant 8(e) submission based on EPA's reporting guidance. 3M appreciates EPA's attention to this matter. Please contact the undersigned if you have any questions or require further information regarding this submission. I11HIIIIH1H1 EHQ 04 Very truly yours, Dr. Katherine E. Reed, Ph.D Staff Vice President Environmental Technology and Satisfy Services (651) 778-4331 kereed@mmm.com CO 88040000348 88040000342 Master Index to Studies Submitted Under TSCA 8(e) by 3M Company on September 24, 2004 (Confidential Business Information Redacted) Primary Eye Irritation Study - Rabbits I J[ 20% solids (Ethomeen S/12 1.0M with diethyl 1 sulfate 0.94M); 80% water [Ethomeen S/12 * R- Guinea Pig Contact Dermal N(Et)+(C2H40H)2 where R=C18 with 1-2 Irritation/Sensitization double bonds] 20% (61791-24-0 with 64-67-5); 80% 7732-18-5 Primary Eye Irritation Study - Rabbits Butanoic acid, heptafluoro-, calcium salt 2366-98-5 Acute Oral Toxicity Screen with T- 2712CoC in Albino Rabbits perfluorohexanoic acid 307-24-4 Primary Skin Irritation Test with T- 2725Ec (Repeat Application) in Albino Rabbits 1 Acute Ocular Irritation Test with T- ][ I 2725Ec in Albino Rabbits t Sensitization Study with T-2741AC 1l 1 in Albino Guinea Pigs [... - 1[ Oral Rangefinder Study of T-3140BS 1-[3'-{perfluorooctanesulfonate) anilino amide]-2 I in Pregnant Rats potassium 3,4,5,6-tetrachlorophthalate 57589-85-2 80% 1-[3'-(perfluorooctanesulfonate) anilino amide}-2-potassium 3,4,5,6- Oral Rangefinder Study of T-3139BS tetrachlorophthalate: 5% C7 homolog; 5% C5 80% 57589-85-2; 5% 68541-01-5 ; 5% 68541-02-6; in Pregnant Rats homolog: 5% C4 homolog; 5% C6 homolog 5% 68568-54-7; 5% 68815-72-5 Acute Occular Irritation Test with T- perfiuoroethylcyclohexylsulfonic acid diethanol 2997CoC in Albino Rabbits amine salt salt of 133201-07-7 and 111-42-2 Sensitization Study with T-3386 in Albino Guinea Pigs [ ]n Vitro Microbiological Mutagenicity ]t l Assays of 3M Company's Compound T-3411 I _________________________________ ]______ [ 1 Vi 1 Master Index to Studies Submitted Under TSCA 8(e) by 3M Company on September 24, 2004 (Confidential Business Information Redacted) 68% poly(oxy-1.2-ethanediyl), alpha-[2- [ethyl[(heptanedecanuoroocty!)sulfonyl]amino]et hyl]-omega-hydroxy-; 12% polethylene glycol; 7% water; 4.86% poly(oxy-1,2-ethanediyl), alpha-[2- [ethyl[(pentadecafluoroheptyl)sulfonyl)aminoJeth yl]-omega-hydroxy-; 4% residual organic fluorochemical; 3% heptadecafluoro-1- octanesulfonic acid; 0.81% poly(oxy-1,2- ethanediyl), alpha-[2- [ethyl[(undecafluoropentyl)sulfonyl]aminojethyl]- omega-hydroxy-; 0.3% 1,4-dioxane; 0.2% n- 68% 29117-08-6; 12% 25322-68-3; 7% 7732-18-5; elhylperiluorooctanesulfonamidoethyl alcohol; 4.86% 56372-23-7; 4.05% 68298-79-3; 3.24% Acute Oral Toxicity Screen with T- 0.03% linear n-ethyl 68298-81-7; 3% 1763-23-1; 0.81% 68298-80-6; 3448 in Albino Rats perfluorooctanesulfonamide 0.3% 123-91-1; 0.2% 1691-99-2; 0.03% 4151-50-2 In Vitro Microbiological Mutagenicity Assays of 3M Company's Compound T-3516 l Acute Dermal Toxicity Study with T- J[ I 3451 in Albino Rabbits C 8F 17S 0 2N (C H 3 ).N a Unknown Acute Oral Toxicity - Method, Summary, Pathology; Primary Dermal Irritation - Method. Summary; Primary Eye Irritation - Method, Summary; Guinea Pig Maximization - Method, Summary Acute Oral Toxicity - Method, [ ][ I Summary, Pathology: Primary Dermal Irritation - Method, Summary; Primary Eye Irritation - Method, Summary; [ J[ 1 Dermal Sensitization Study in [ I[ I Guinea Pigs, Maximization Test - Method, Summary I 1[ ] 4 Hour Acute Aerosol Inhalation [ I[ ] Toxicity Study with T-3825 in Rats [ Primary Eye Initaiton/Corrosion 1[ J Study in Rabbits 4-Hour Acute Aerosol Inhalation 1 J[ ] Toxicity Study with T-3825 in Rats I_________________________________ 1 I_________________________________ 1_________ 2 Master Index to Studies Submitted Under TSCA 8(e) by 3M Company on September 24, 2004 (Confidential Business Information Redacted) T-3820: Acute Inhalation Toxicity Test T-3821: Acute Inhalation Toxicity Test T-3845 Acute Inhalation Toxicity Test Evaluation of the Acute Inhalation Toxicity of T-3920 in the Rat Primary Eye Irritation Study in Rabbits - Method, Summary Acute Oral Toxicity Study in Rats (OECD Guidelines) Acute Inhalation Toxicity Study with T-4129 in the Rat Acute Inhalation Toxicity Study with T-4130 in the Rat Acute Oral Toxicity Study in Rats; Acute Dermal Irritation Study in Rabbits; Acute Eye Irritation Study in Rabbits Dermal Sensitization Study in Guinea Pigs - Maximization Test 1 l heptafluorobutyryl chloride l ] t) Decanoic add, nonadecafiuoro-, ammonium salt 95% ammonium periluorodecanoate; 5% ammonium periluorooctanoate [1 I1 [] I1 1 [ 375-16-6 [ 3108-42-7 5% 3825-26-1 [ I [ [ I ] ] 1 ] ] ] Mutagenicity Test on T - 4413 [ ) Mouse Lymphoma Forward Mutation Assay with Duplicate Cultures [ Acute Inhalation Toxicity Study with 1[ ] T-4354 in the Rat [ Primary Dermal Irritation/Corrosion 1[ l Study in Rabbits Acute Inhalation Toxicity Study in [ 1[ l the Rat with T-4397 Primary Eye Irritation/Corrosion I 1[ ] Study of T-5261 in Rabbits lithium tetrafluoroethane-1,2-disulfonimide Unknown Acute Inhalation Toxicity Evaluation on T-5231 in Rats 4-Hour, Acute Inhalation Toxicity I_________________________________ l I 1 Study with T-5305 in Rats 4-Hour, Acute Inhalation Toxicity i l[ I Study (Limit Test) with T-5343.1 in Rats I_________________________________ I______ I_________________________________ 1 3 Master Index to Studies Submitted Under TSCA 8(e) by 3M Company on September 24, 2004 (Confidential Business Information Redacted) 4-Hour. Acute Inhalation Toxicity Study With T-5306 in Rats 4-Hour, Acute Inhalation Toxicity [ I Study (Limit Test) with T-5357.1 [ Acute Dermal Toxicity Study of T- I 4201 in Rabbits Lithium Bis(Trifluoromethanesulfonyl)imide SubAcute 28-Day Oral Toxicity with T-2816 by Daily Gavage in the Rat Followed by a 14 Day Recovery Period [ Subacute 28-Day Oral Toxicity with ] T-2816 by Daily Gavage in the Rat Followed by a 14-Day Recovery Period I Acute Inhalation Toxicity Evaluation J on T-5187 in Rats [ T-4240 4-W eek Oral Toxicity Study l in Rats Dermal Sensitization Study of T- l 1 5473 in Guinea Pigs - Maximization Test 4-Hour. Acute Inhalation Toxicity [ ] Study With T-5698 in Rats t Acute Inhalation Toxicity Evaluation 1 On T-5708 in Rats T-5486 Assessment of Cardiac [ ] Sensitization Potential in Dogs octafluoropropane Acute Inhalation Toxicity Evaluation on T-5655 in Rats [ T-4201 4 Week Oral Toxicity Study 1 in Rats with 2-W eek Recovery Period Lithium Bis(Trifluoromethanesulfonyt)imide T-5658: Eye Irritation to the Rabbit t Acute Inhalation Toxicity Evaluation I onT-5715in Rats 1 Acute Inhalation Toxicity Evaluation I on T-5716 in Rats [ Acute Inhalation Toxicity Study of T- 1 5724 in Rats [ Acute Inhalation Toxicity Study of T- J 5725 (Resin Solution) in Rats I _________________________________ ]_____ I [ 90076-65-6 1 ] [I (1 I] I1 l [ I 76-19-7 t ] 1 ] ] 90076-65-6 t 1 [I [I [I I_________________________________ l 4 Master Index to Studies Submitted Under TSCA 8(e) by 3M Company on September 24, 2004 (Confidential Business Information Redacted) Acute Inhalation Toxicity Study (Limit Test) of T-5927 in Rats I Acute Inhalation Toxicity Study of T- 5928 in Rats (LC50) I Acute Inhalation Toxicity Evaluation on T-5829 in Rats Single-Dose Intravenous i Pharmacokinetic Study of T-5963 in Rabbits Single-Dose Intravenous [ Pharmacokinetic Study of T-6030 in Rabbits I l[ l[ It I[ I[ I 1 1 ] 1 87-93% fluorinated alkyl alkoxylates; 4-10% linear N-ethyl perfluorooctanesulfonamide; 2- 4% poly(oxy-1,2-ethanediyl),,alpha.-[2- [ethyl[(pentadecafluoroheptyl)sulfonyl]aminoleth yi]-.omega.-methoxy-; 0-4% residua) organic fluoFochemicals; 0-2% c8 sulfonamide; 0.1-1% 5-Daily Dose Dermal 1-heptanesulfonamide, N-ethyl- Absorption/Toxicity Study of T-6029 1,1,2,2,3.3,4,4,5.5,6,6,7,7,7-pentadecafluoro-; 87-93% 68958-61-2; 4-10% 4151-50-2; 2-4% and T-6032 in Rabbits miscellaneous components (each less than 1%) 68958-60-1; 0-2% 31506-32-8; 0.1-1% 68957-62-0 Single-Dose Intravenous Pharmacokinetic Study of T-6061 in Rabbits Single-Dose Intravenous [ ][ ] Pharmacokinetic Study of T-6065 in Rabbits Single Dose Intravenous [ 1( I Pharmacokinetic Study of T-6063 in Rabbits l Acute Inhalation Toxicity Study of T- 1l 1 6235 in Rats [ Primary Dermal trritation/Corrosion 1[ ] Study of T-6402 in Rabbits [ JI I Dermal Sensitization Study of T- 6402 in Guinea Pigs- Maximization Test (EC Guidelines) [ 1 Acute Eye Irritation/Corrosion Study 1-Bulanesulfinic acid, 1,1,2,2,3,3,4,4,4- with T-6318 in the Rabbit nonafluoro-, Sodium Salt [ 102061-82-5 1 5 Master Index to Studies Submitted Under TSCA 8(e) by 3M Company on September 24, 2004 (Confidential Business Information Redacted) Primary Skin Irritation / Corrosion Study with T-6567 in the Rabbit (4- Hour Semi-Occlusive Application) [ Assessment of Contact 1 Hypersenitivity to T-6318 in the Albino Guinea Piq (Maximization 1-Butanesulfinic acid, 1,1,2,2,3,3,4,4,4- Test) nonafluoro-. Sodium Salt Single-Dose Intravenous Pharmacokinetic Study of T-6502 in Rabbits Single-Dose Intravenous t 1 Pharmacokinetic Study of T-6504 in Rabbits Single Dose Intravenous [ 1 Pharmacokinetic Study of T-6506 in Rabbits [ A Study for Effect on Embryofoetal 1 Development of the Rat (Inhalation 20-80% methyl nonafiuoroisobutyl ether; 20- Administration) 80% methyl nonfluorobutylether Bacterial Reverse Mutation Test of T 6695 5-day Inhalation Toxicity of [ ] Perfluorocyclohexene ([ ]; T- 70% crude perfluorocyclohexene; 30% 6878) in Rats periluoromethylcyclopentene 5-Daily Dose Dermal Absorption/Toxicity Study of T-6502 and T-6503 in Rabbits Primary Eye Irritation/Corrosion [ 1 Study of T-6786 in Rabbits Lithium Bis(perfluoroethylsu!fonyl)imide Primary Dermal Irritation/Corrosion Study of T-6804 in Rabbits Lithium Bis(perfluoroethylsulfonyl)imide 5-Day Inhalation Toxicity Screen of HFE[ l C-C6F110CH3 Primary Eye Irritation/Corrosion Study of T-6804 in a Rabbit (OECD Guidelines) Lithium Bis(perfiuoroethylsulfonyl)imide Acute Oral Toxicity Study of T-6804 in Rats (OECD Guidelines) Lithium Bis(perfluoroethylsulfonyl)imide Dermal Sensitization Study of T6908 in Guinea Pigs, Mazimization Test (EC Guidelines) 11 102061-82-5 t] t1 [1 20-80% 163702-08-7, 20-80% 163702-07-6 [J 70% 355-75-9 [ 132843-44-8 132843-44-8 4943-08-2 132843-44-8 132843-44-8 ] 6 Master Index to Studies Submitted Under TSCA 8(e) by 3M Company on September 24, 2004 (Confidential Business Information Redacted) Eye Irritation/Corrosion Study of T- N-Me Fos Amide-Triphenylbenzyl Phosphonium 4127 in the Rabbit Chloride Complex; D-1624 31506-32-8 Single-Dose Intravenous Pharmacokinetic Study of T-6924 in Rabbits [ ][ l Dermal Sensitization Study of T6924 in Guinea Pigs- Maximization Test (EC Guidelines) [ Jt ] Dermal Sensitization Study of T- 7003 in Guinea Pigs - Maximization Test (EC Guidelines) [ Report of Sera and Liver Data for ( N-ethyl heptadecafluoro-N[2- 1[ 1 ] Monoester - Preliminary ADME (phosphonooxy)ethyl] octanesulfonamide Study in Rats diammonium salt 67969-69-1 [ ] Diester-Pharmacokinetic Study in Rats (Study No. T-7043.1, ammonium DT-26) bis(ethyl(periluorooctane)suifonayl]phosphate 30381-98-7 Single Dose Intravenous Pharmacokinetic Study with T-7082 in Rabbits t N-ethyl heptadecafluoro-N[2- ]( ] [ ] Monoester - Pharmacokinetic (phosphonooxy)ethyl] octanesulfonamide Study in Rats (Study No. T-6997.2) diammonium salt 67969-69-1 Determination of PFOS Presence and Concentration in Serum from the Dermal Absorption Studies of T- 7106 and T-7107 in Hra:(NZW)SPF Rabbits Dermal Sensitization Study of T- [ 1 1. 1 7285.5 in Guinea Pigs - Maximization Test (EPA/OECD Guidelines) l Twenty-eight Day Repeated-Dose .] l 1 Oral Toxicity Study of T-6861 in Rats Lithium Bis(perfluoroethylsulfonyl)imide 132843-44-8 Twenty-eight Day Repeated Dose Oral Toxicity Study of T-7005 in Rats I_________________________________ 1______ I_________________________________ L 7 Master Index to Studies Submitted Under TSCA 8(e) by 3M Company on September 24, 2004 (Confidential Business Information Redacted) Acute (4-Hour) Inhalation Toxicity of Test Atmospheres Obtained after Heating [___________ 1in Rats f_________________________________ ]______ Toxicokinetic Study of Perflurooctanesulfonamidoacetate ([ ]; T-7071.2) in Rats perfluorooctanesulfonamido carboxylic acid 2806-24-8 Acute Nose-Only Inhalation Toxicity Study of T-7087, T-7088, T-7089 and T-7090 in Rats (Limit Test) I______________________ I l .. Acute Ocular Irritation Study of T- ... 1 7485 Applied to New Zealand White Rabbits potassium nonafluorobutanesulfonate Toxicokinetic Study of Perfluorooctane Sulfonamide (PFOSA, T-7132.2) in Rats perfluorooctanesulfonamide Acute Four-Hour Inhalation Study in Perflurobutanesulfonyl Fluoride (96-98% ) And Rats Perfiuorosulfolane (2-4% ) Frimary Eye Irritation/Corrosion Study of T-7508.2 in Rabbits MV31 K-Salz; Test for Primary [ ] Dermal Irritation in the Rabbit [ Assessment of Acute Oral Toxicity J with T-7560 In The Rat (Acute Toxic Class Method) f Acute Eye Irritation/Corrosion Study 1 with T-7560 in the Rabbit l J [ ] Potassium bis- (perfluorobutanesulfonyt)imide Repeat Dose ADME Study in Rats Potassium bis(perfluorobutanesulfonyl)imide Toxicity Study by Repeat Dose Inhalation Administration to CD Rats Perflurobutanesulfonyl Fluoride (96-98% ) And for 4 Weeks Perfiuorosulfolane (2-4% ) [ l 29420-49-3 754-91-6 96-98% 375-72-4; 2-4% 42060-64-0 I t [ t 129135-87-1 96-98% 375-72-4; 2-4% 42060-64-0 ] I ] ] ] 1 A Sub-acute( 28 Day) Inhalation Toxicity Study, Including a Recovery 1.1,1,2,2,4,5,5,5-nonafluoro-4-(trifluoromethyl)-3 Study, with T-7479 in Rats pentanon 756-13-8 Xenochemical Receptor trans- Activation by Perfluorooctane-based Chemicals perfluorooctanesulfonamide 754-91-6 8 Master Index to Studies Submitted Under TSCA 8(e) by 3M Company on September 24, 2004 (Confidential Business Information Redacted) 84% 1-octanesulfonicadd, 1.1,2,2.3,3,4,4,5,5,6,6,7,7,8,8,8- heptadecafluoro-, potassium salt; 5.5% potassium (perfluorohexyl)sulfonate; 4% potassium nonafluorobutanesulfonate; 4% potassium periluoroheptanesulfonate; 2% potassium periluoropentanesutfanate, 0.5% 84% 2795-39-3; 5.5% 3871-99-6; 4% 29420-49-3; unknown 4% 60270-55-5; 2% 3872-25-1 95% N-ethylperfluorooctanesulfonamidoethyl alcohol; 5% 1-heptanesulfonamide N-ethyl- 1,1,2,2,3,3,4,4 .5 .5 ,6 .6,7,7,7-p en tadecafluoro-N- (2-hydroxyethyl}- 95% 1691-99-2; 5% 68555-73-7 Acute Inhalation Toxicokinetic Study of Periluoroctartesulfonyl Fluroide (POSF) T-7098.4 periluorooctanesulfonyl fluoride 307-35-7 Five-Day Inhalation Toxicity Study of HFE [ ] in Male CD Rats C-C6F11-CF2-0-CH3 181214-67-5 Acute Toxicity Screen of Perfluorocyclohexene (T-6878) in 70% crude perfluorocyclohexene; 30% Rats perfluoromethylcyclopentene 70% 355-75-9 [ 1 (T-7056) Toxicokinetic Study in Rats l l l ......... N-Methyl Perfluorobutylsulfonamide = 95% 1- ] Assessment of Acute Oral Toxicity Butanesulfonamide, 1,1,2,2,3,3.4,4,4- with T-7601.3 in the Rat (Acute Nonafluoro-n-Methyl; 5% N-Methyl-4-Hydrido- Toxic Class Method) Perfluorobutylsulfonamide 68298-12-4 Subchronic 90-Day Oral Toxicity Study with T-7320 By Daily Gavage in the Rat Followed by a 28-Day Recovery Period l ... I[ ] 84% 1-octanesulfonic acid, Protein Binding of Perfluorobutane 1,1,2,2,3,3.4.4,5,5,6,6,7,7.8,8,8- Sulfonate, Perfluorohexane heptadecafluoro-, potassium salt: 5.5% Sulfonate, Perfluorooctane Sulfonate potassium (perfluorohexyl)sulfonate; 4% and Perfluorooctanoate to Plasma potassium nonafluorobutanesulfonate; 4% (Human, Rat, and Monkey), and potassium perfluoroheptanesulfonate; 2% Various Human-Derived Plasma potassium perfluoropentanesulfanate; 0.5% Protein F ractions unknown potassium nonafluorobutanesulfonate potassium (peri!uorohexyl)sulfonate 84% 2795-39-3; 5.5% 3871-99-6; 4% 29420-49-3; 4% 60270-55-5; 2% 3872-25-1 29420-49-3 3871-99-6 V9 Master Index to Studies Submitted Under TSCA 8(e) by 3M Company on September 24, 2004 (Confidential Business Information Redacted) potassium periluorooctanoate Five Day Inhalation Toxicity Study of [ ] Monochloride, [ ], and HCFC225cb in Male CD Rats C4F9-OCH2CI c-C6F 11-CF2-0-CH3 CF2CICF2CHCIF Toxicokinetic Screen of I ] (T- 7483) in Rats C 7 F 1 5C (0 )N (H )C H 3 84% 1-octanesulfonicacid, 1,1,2.2,3,3,4,4,5,5,6,6,7,7,8,8.8- heptadecafluoro-, potassium salt; 5.5% potassium (perfluorohexyl)sulfonate: 4% Low Level Oral potassium nonafluorobutanesulfonate; 4% Periluorooctanesulfonate (PFOS) potassium periluoroheptanesulfonate; 2% Dose Toxicokinetic Study in Rats: potassium periluoropentanesutfanate; 0.5% Serum and Liver PFOS unknown 2395-00-8 205367-42-6 (n-isomer) and 221617-86-3 (1isomer) 181214-67-5 507-55-1 89685-56-3 84% 2795-39-3; 5.5% 3871-99-6; 4% 29420-49-3; 4% 60270-55-5; 2% 3872-25-1 10 CONFIDENTIAL BUSINESS INFORMATION SUBJECT TO PROTECTION UNDER THE TOXIC SUBSTANCES CONTROL ACT AND OTHER LAWS HAS BEEN REDACTED FROM THIS DOCUMENT FINAL REPORT Study Title: Toxicokinetic Study of Perfluorooctane Sulfonamide {PFOSA; T-7132.2) in Rats Authors: Andrew M. Seacat Ph.D. Toxicology Specialist 3M Medical Department, Corporate Toxicology Deanna J. Luebker M.S. Advanced Toxicologist 3M Medical Department, Corporate Toxicology Date: August 11, 2000 Testing Facility 3M Strategic Toxicology Laboratory 3M Center 270-3 S-05 Saint Paul, MN 55144 3M Strategic Toxicology ST39 T-732.2 PFOSA PK study in rats Summary: Purpose: The purpose o f this study was to assess the relative absorption, metabolism, and elimination kinetics o f Perfluorooctane Sulfonamide (PFOSA) in the rat following a single oral dose. Methods: Two groups of fifteen male rats each received a single dose o f either 2% Tween 80, as the vehicle control, or 5 mg/kg PFOSA suspended in 2% Tween 80 by oral gavage. Perfluorooctanoate (POAA) was found at a level of 2.5 ng/ml in the dosing solution. The PFOSA was found to be 96 % pure Five rats from each dose group were sacrificed on days 1,4, and 29 post dose. Liver and sera were analyzed for PFOSA and its predicted metabolites using highpressure liquid chromatography/electrospray tandum mass spectrometry (HPLC/ESMSMS). Results: The vehicle control group had no detectable levels o f PFOSA or perfiuorooctanesulfonate (PFOS) in liver or sera. The PFOSA dose group had decreasing levels of PFOSA, with evidence of conversion of PFOSA to PFOS in liver and sera throughout the study. Liver concentrations of PFOSA averaged 7.0 ppm, 3.7 ppm, and 0.1 ppm on days 1, 4, and 29 post-dose, respectively, with an apparent liver half-life of elimination of 5.2 days. Serum concentrations of PFOSA averaged 0.3 ppm and 0.1 ppm on days 1 and 4 post dose respectively, and were undetectable by day 29 post-dose, with an apparent serum half-life of elimination estimated to be less than 4 days. Liver PFOS concentrations were 28.2 ppm, 37.4 ppm and 23.8 ppm, representing 22.0%. 32.3%, and 25.2% of the PFOSA dosed, on days 1, 4 and 29 post-dose respectively. Sera PFOS averaged 8.2 ppm, 8.6 ppm, and 4.6 ppm on days 1,4 and day 29 post dose respectively. The average total concentrations of PFOS equivalents (PFOS + PFOSA) in liver were 35.2, 41.1, and 23.9 ppm on days 1,4, and 29 post-dose, respectively. The average concentrations of PFOS equivalents in the sera increased from 8.5 ppm on day 1 post dose to 8.7 ppm on day 4 post dose and decreased to 4.6 ppm on day 29 post dose. The liver to sera PFOS concentration ratio increased throughout the study with values of 4.2, 4.8, and 5.4 on days 1,4, and 29 post dose, respectively. Total PFOS equivalents in the liver and sera peaked on day 4 post dose at 35.4% and 6.0 % of the PFOS equivalents dosed, respectively. An average of 0.1 ppm POAA was found in the sera on day 1 and day 4 post dose, and equaled 31.2% and 24.l% of the POAA residual present in the dose, respectively. Conclusions: Perfluorooctanesulfonamide was readily absorbed from the gut and found in the liver and sera following an oral exposure. PFOSA was progressively metabolized to PFOS, which accumulated in the liver as evidenced by the high concentration o f PFOS detected in the liver, representing 22.0% 32.3% and 25.2% of the PFOSA dosed, on days 1,4 and 29 post dose respectively. The apparent half-live of elimination of PFOSA in the liver was approximately 5.2 days. The POAA present in the sera on days l and 4 post-dose could be accounted for by the residual POAA in the dosing solution, therefore, no direct evidence for metabolism of PFOSA to POAA was found in this study. Page 2 of 18 T39 T-7132.2 PFOSA PK study ut rats CONFIDENTIAL BUSINESS INFORMATION SUBJECT TO PROTECTION UNDER THE TOXIC SUBSTANCES CONTROL ACT AND OTHER LAWS HAS BEEN REDACTED FROM THIS PAGE Introduction The objective of this study was to assess the potential for oral.absorption, urinary and fecal clearance, and biological persistence o f Perfluorooctanesulfonamide (PFOSA) in male Sprague Dawley rats after a single oral dose. Analysis of the serum and liver for PFOSA and potential metabolites of PFOSA was performed by LCMS. Urine and feces were also collected and may be analyzed by LCMS and perhaps other methods as deemed necessary. Previous studies on N-ethylperfluoroctanesulfbnamide (1), the N-ethyl derivative of PFOSA, mistakenly concluded that PFOSA was the ultimate metabolite in rats (1,2); however, the gas chromatography analytical technique used in those studies was unable to detect PFOS. Dietary administration o f N-ethylperfluoroctanesulfonamidoethano! (N-EtFOSE) in rats, and in-vitro metabolism by hepatocytes results primarily in the formation of PFOS with a minor amount of PFOSA (3, 4, and 5). Furthermore, PFOSA has been identified as a potent direct uncoupler of mitochondrial respiration in-vitro (6). Prior to the current study, direct metabolism o f PFOSA to PFOS had not been demonstrated and the relative toxicokinetics o f PFOSA were unknown. Methods were recently validated for the quantitation of PFOSA and its potential metabolite, PFOS, in serum and liver down to the low part per billion level (7). In-vivo studies were, thus, warranted to investigate the toxicokinetics of PFOSA. Materials _ The test material was identified as Perfluorooctanesulfonamide (PFOSA)! initial analysis by GCMS determined that the staring material was over 99% pure (8). Qualitative' and quantitative compositional results derived from 'H and 19F-NMR analysis revealed that the isomer distribution was approximately 65.8% CF3 (CF2) X-S02-NH2 (Normal chain), 18.7% internal monomethyl branch and 11.2% Isopropyl branch (9). HPLC/MS characterization revealed iow-level impurities of 9,600 ppm PFOS (0.96 %), and lower concentrations of several other amides (10). Perfluorooctanoate (POAA) was found in the dosing solution at a level of 2.5 pg/ml (0.25% o f the nominal dose) (12). Based on the sum of the impurities, the purity of the PFOSA sample was determined to be approximately 96 % (8, 9 & 10). Methods The protocol (11) and analytical methods (12) used in this study are briefly described below. Dose and Dosing Procedures: A single 5mg/kg dose of PFOSA was administered via oral gavage to 15 male Sprague Dawley rats (obtained from Harlan Laboratories) on day zero of the study. The PFOSA was prepared as a 1% (I mg/ml) uniform suspension in 2% Tween 80. A volume of 5 ml suspension / kg body weight was administered to each rat. The vehicle control group, consisting of 15 male Sprague Dawley rats (also obtained from Harlan Laboratories), received 2% Tween 80 in deionized water at a volume o f 5 ml/kg on day zero of the study. Page 3 o f 18 3M Strategic Toxicology ST39 T -7132.2 PFOSA PK study In rats Specimen Collection: Urine and feces collections were made on days 1 - 4 post dose from the animals designated for sacrifice on day 29 post dose group. Five animals from each dose group were euthanized by C 02 on days 1,4, and 29 post dose and gross necropsy was performed. Sera and liver were collected from each animal and flash-frozen in liquid nitrogen. Specimen Handling: Specimens (urine, feces, liver, and serum) were maintained at -70C and sent to Kiris Hansen, Ph.D., 3M Environmental Technology and Safety Services, for analysis. Liver and sera samples were analyzed by 3M Environmental for the parent compound and metabolites. The limits of detection (LODs) for PFOSA were 3.5 ng/tnl in the liver and 1.51ng/ml in the sera. The LODs for PFOS were 8.45 ng/ml in liver and 1.74 ng/ml in the sera (12). Urine and feces were retained for possible future analysis as appropriate. Results Control Groups: Body and Liver Weight The average initial body weight SD of the fifteen vehicle control male rats was 273.7 7.3 g. These rats lost an average of 2.2 g body weight from day zero to day 1 post dose . From day zero to day 4 post dose, the average body weight gain was`24.2 g and from day zero to day 29 post dose, body weight increased an average of 114.1 g . Liver weights and relative liver to body weight percentages are shown in Table 1A. Liver and Sera Concentrations Control animals had no detectable levels of PFOSA or PFOS in liver or sera at any time during this study (data not shown). PFOSA Dose Groups: Body and Liver Weight The average initial body weight SD o f the fifteen PFOSA dosed male rats was 270.0 3.6 g. These rats lost an average of 4.5 g body weight from day zero to day 1 post dose . From day zero to day 4 post dose, the average body weight gain was 20.0 g and from day zero to day 29 post dose, body weight increased an average of 100.9 g . Liver weights and relative liver to body weight percentages were equivalent to control values (Table IB). Liver and Sera Concentrations PFOSA and PFOS were detected in the liver and sera o f all animals dosed with. PFOSA. Liver and sera levels of PFOSA were highest on day 1 post dose and dropped significantly between " Page 4 of 18 3M-Strategic Toxicology ST39 T-7132.2 PFOSA PK study in rats days 1 and 4 post dose and again between days 4 and 29 post dose (Tables 2 and 3). The average liver concentrations o f PFOSA decreased from approximately 7.0 ppm to 3.7 ppm to 0.1 ppm from days 1 to 4, to 29 post dose, respectively (Table 2). The half-life of elimination of PFOSA in the liver was calculated from a log linear regression o f the liver PFOSA concentrations to be 5.2 days. The sera concentrations ofPFGSA were 0.3 0.1 ppm, 0.1 0.0 and <LOD (1.74 ng/ml) on days 1, 4, and 29 post dose, respectively (Table 3). The half-life of elimination of PFOSA in the serum cannot be calculated from this data, but is estimated to be less than 4 days. Average PFOS liver and sera levels peaked on day 4 post dose and declined by day 29 post dose to lower levels than found on day one. Average SD liver PFOS levels increased significantly from 28.2 6.1 ppm on day 1 post dose to 37.4 3.6 ppm on day 4 post dose. Levels then decreased significantly to 23.8 4.1 ppm by day 29 post dose (Table 2). Average sera PFOS values were approximately 8 ppm on day 1 and day 4 post dose, then decreased significantly to approximately 4.6 ppm on day 29 post dose (Table 3). Liver and Sera Concentrations as a Percentage of Dose The percentage of PFOSA dosed detected as PFOSA in the liver and sera peaked on day one post dose at 5.4% and 0.2 % respectively. By day 4 post dose, these levels had dropped to 3.2% and 0.0 % and by day 29 post dose the liver levels dropped to 0.1 % and the sera levels remained at 0.0% (Table 6). The percent PFOS equivalents dosed detected as PFOS in the liver and sera was 22.0% and 5.2 % on day l post dose and increased to 32.3% and 6.0% by day 4 post dose. On day 29 post dose, these levels had dropped to 25.2% and 4.1%, respectively (Table 6). Residual PFOS in the dose could account for 3.5%. 2.5%, and 5.6% of the PFOS found in sera, and 3.6%, 2.7%, and 3.9 % of the PFOS found in liver on days 1,4, and 29 post dose, respectively (Tables 4 and 5). The percent PFOS equivalents dosed detected as PFOS equivalents in the liver and sera was 27.2 % and 5.3 % n day 1 post dose and increased to 35.4 % and 6.0 % by day 4 post dose. On day 29 post dose these levels decreased to 25.4 % and 4.1 % in the liver and sera respectively (Table 6). Sera POAA Concentrations Perfluorooctanoaie (POAA) was found at a level o f 2.5 ng/ml in the dosing solution (12). Sera samples in the PFOSA dose group contained POAA at average values of 0.1 and 0.8 ppm POAA on days 1 and 4 post-dose respectively. These values equal 30.8% and 23.5%, respectively, of the POAA dosed (Table 7). Conclusions: No compound related effects were observed on body weight, liver weight, or liver/body weight ratios under treatment conditions. Both PFOSA and PFOS were found at high concentrations in the liver and sera of rats one day following an oral dose. Approximately 38% of the PFOSA dosed was converted to PFOS four P age 5 o f 18 3M 'Strategic Toxicology ST39 T-7132J2 PFOSA PE study in rats days post-dose. PFOSA levels diminished in both sera and liver over time, with a liver half-life of approximately 5.2 days, and a much shorter residence period in the sera. Significantly more PFOS was found in the liver and sera at all time points than were present in the dose, therefore metabolic conversion of PFOSA to PFOS occurred. No direct evidence for metabolism of PFOSA to POAA was found in this study. The route o f elimination of PFOSA in this study was not determined. No glucuronide or other conjugates were analyzed for, and further investigation of possible conjugates in the urine and feces is warranted. It is possible that some of the PFOSA was eliminated through the lung via expiration, but this has not been determined. The present results suggest that the PFOSA from the dose is progressively converted to PFOS and that the resulting PFOS is accumulated in the Liver. Page 6 o f 18 3M-Strategic Toxicology ST39 T-7132.2 PFOSA PK study inrats Report Prepared by: Signatures Deanna Luebker, MS7 Advanced Research Toxicologist V , Andrew M. Seacat, Ph.D. Toxicology Specialist Report Reviewed by: John L. Butenhoff, Ph.D., DABT, CIH Senior Laboratory Manager .... O l/ilo / m o / Date o r / u > i t Date / JTW Date O/ Page 7 o f 18 3M Steateglc Toxicology ST39 T-7132.2 PFOSA PK study in rats References: CONFIDENTIAL BUSINESS INFORMATION SUBJECT TO PROTECTION UNDER THE TOXIC SUBSTANCES CONTROL ACT AND OTHER LAWS HAS BEEN REDACTED FROM THIS PAGE 1. Grossman M.R. and Bowen J.M, (1990) Tissue analysis o f fluorinated sulfonamide pesticide: an evaluation of distribution, elimination, and potential for bioaccumulation in orally exposed rats, M.S. Thesis, Univ. of 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. Fimdam. Appi 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. Mulvana D.E. and Henion J. 1996. Qualitative investigation o f the in-vitro metabolism of T6292, T-6293, T-6294 and T-6295 by rat and human hepatocytes using ion spray LC/MS and LC/MS/MS. Analytical Report: 96ADEM01.3M, Advanced Bioanalytical Services, Inc. 45pp. 4. Poon G.K., Lowes S. 1998. Additional Characterization of metabolites of T-6292, T-6293 and T-6294 from rat and human hepatocytes by TurboIonSpray LC/MS and LC/MS/MS. Semi-quantitative analysis of T-6295 in rat and human hepatocytes incubated with T-6292, T-6293 and T-6294 by LC/MS/MS. Analytical Report: 96AGKP1.3M, Advanced Bioanalytical Services, Inc. 69pp. 5. Seacat A.M., Thomford P.J., Hansen K J. and ButenhofT J.L. Sub-Chronic Dietary N-Ethvl Perfluorooetanesulfonamido Ethanol Toxicity in Rats, (in preparation, 8/11/2000). 6. Wallace K.B. and Starkov A. 1998. The effect of perfluorinated arylalkylsulfonamides on bioenergetics of rat liver mitochondria. Dept, of Biochemistry and Molecular Biology, University of MN School of Medicine. Duluth, MN 55812, USA. Supported by a grant front 3M Company 7. K.J. Hansen, L.A. Clemen, M.E. Ellefson, H.O. Johnson, (1999). Compound Specific Characterization of Organic Fluorochemicals in General Population Human Sera Samples. 3M Environmental Lab, St. Paul, MN 55133. 8. Payfer R.M. GC/MS analysis of PFOS . SA&C Analytical Request No. 59426. Report 9/24/99. 3M SA&C Lab Building 236-2B-1. 9. Tom Kestner. Chemical Characterization of PFOSA ^ ty lH and 19F-NMR Spectroscopy Requests # 59426. 3M Specialty Adhesives & Chemicals Analytical Laboratory / SMMD-236-2B-11, September 25, 1999. p -j 10. DeRoos F.L. Characterization of PFOSA Samples, T-7132-l/ Jtnd TN-A-1584. Request # A-151254. Report 10/7/99. Corporate Analytical Technology Center, Building 201-1-29, CATC - Chromatography Group. Page 8 o f 18 3MStrategic Toxicology ST39 T-7132.2 PFOSA PK study in rats 11. Seacat & Luebker. Protocol for Study No. T-7132.2; ST-39, PHARMACOKINETIC STUDY OF PFOSA IN RATS. 3M Medical Department, Corporate Toxicology. October 1999. 12. Laboratory Report: Analytical Report of Data for PFOSA (T-7132.2) Pharmacokinetic Study in Rats (Sera and Liver). Laboratory Report No. FACT-TOX-145 (W2814). Testing Laboratory 3M Environmental Technology' & Safety Services, 3M Environmental Laboratory', Fluorine Analytical Chemistry' Team. Laboratory Contact: Kris Hansen, Ph.D. 13. Aiman and Dittmer, Blood and Other Body Fluids. FASEB, 1971, p5 P age 9 o f 18 3M Strategic Toxicology ST39 T-7132.2 PFOSA PK study in rats List of Tables: Table 1: Biological Parameters 1A: Control Group IB: PFOSA Dose Group. Table 2: Liver PFOSA and metabolites in the PFOSA Group. Table 3: Serum PFOSA and metabolites in the PFOSA Group Table 4: Percent Dose: Liver PFOS equivalents in PFOSA Group. Table 5: Percent Dose: Serum PFOS equivalents in PFOSA Group. Table 6: Summary; Percent of dose in sera and liver. Table 7: Serum POAA in the PFOSA Group. 3M Strategie Toxicology ST39 T-71322 PFOSA PK study in rats Table 1A: Biological Parameters. Control Group Time Dose animal # Initial Terminal BW Gain Liver Liver wt as 9R03-XXX BW(g) BW(g} (9> w tis) %of BW Day 1 Control 230 282.5 282.0 -0.5 12.0 4.3% Day 1 Control 231 272.1 268.4 -3.7 11.2 4.2% Day 1 Control 232 277.4 277.1 -0.3 12.4 4.5% Day 1 Control 233 274.1 274.8 0.7 11.5 4.2% Day 1 Control 234 267.6 260.5 -7.1 11.2 4.3% Avg 274.7 272.6 -2.2 11.7 4.3% SD 5.6 8.3 3.2 0.5 0.1% Day 4 Control 235 266.9 294.5 27.6 11.6 3.9% Day 4 Control 236 275.8 301.8 26.0 11.4 3.8% Day 4 Control 237 261.9 283.4 21.5 11.9 4.2% Day 4 Control Day 4 Control 238 279.0 239 268.3 302.7 291,2 23.7 11.3 22.9 10.7 3.7% 3.7% Avg 270.4 294.7 24.3 11.4 3.9% SD 6.9 8.0 2.4 0.4 0.2% Day 29 Control 240 273.5 371.8 98.3 13.9 3.7% Day 29 Control 241 270.5 380.5 110.0 14.4 3.8% Day 29 Control 242 280.2 389.4 109.2 14.2 3.6% Day 29 Control 243 289.9 444.0 154.1 17.5 3.9% Day 29 Control 244 266.3 365.2 98.9 14.3 3.9% Avg 276.1 390.2 114.1 14.9 3.8% SD 9.2 31.4 23.0 1.5 0.1% Page 11 o f 18 3M Strategie Toxicology ST39 T -7t32,2 PFOSA PK study in rats Table 18: Biological Parameters. PFOSA Dose Group Time Dose animal # Initial Terminal BW Gain Liver Liver wt as 9R03-xxx BW (g) BW(g) () wtfg) % of BW Day 1 5 mg/kp 245 263 2 257.8 -5.4 10.4 4.0% Day 1 5 mg/kg 246 266.1 259.2 -6.9 10.2 3.9% Day 1 5 mg/kg 247 266.5 264.1 -2.4 10.9 4.1% Day 1 5 mg/kg 248 267.2 264.0 -3.2 10.1 3.8% Day 1 5 mg/kg 249 268.7 264.3 -4.4 10.7 4.0% Avg 266.3 261.9 -4.5 10.5 4.0% SD 2.0 3.1 1.8 0.3 0.1% Day 4 5 mg/kg 250 266.6 286.3 19.7 11.3 3.9% Day 4 5 mg/kg 251 272.1 294.6 22.5 11.7 4.0% Day 4 5 mg/kg 252 271.7 294.5 22.8 12.1 4.1% Day 4 5 mg/kg 253 271.8 291.4 19.6 11.3 3.9% Day 4 5 mg/kg 254 272.9 288.4 15.5 11.7 4.1% Avg 271.0 291.0 20.0 11.6 4.0% SD 2.5 3.7 2.9 0.3 0.1% Day 29 5 mg/kg 255 275.2 385.4 110.2 16.7 4.3% Day 29 5 mg/kg 256 273.6 380.3 106.7 14.4 3.8% Day 29 5 mg/kg 257 271.4 373.9 102.5 13.9 3.7% Day 29 5 mg/kg 258 274.5 371.4 96.9 14.6 3.9% Day 29 5 mg/kg 259 268.7 356.7 88.0 12.7 3.6% Ayg 272.7 373.5 100.9 14.5 3.9% so 2.6 10.9 8.7 1.5 0.3% Page 12 o f 18 3M Strategic Toxicology ST39 T-7132.2 P F 05A PK study in rats Table 2: liv e r PFOSA and m etabolites in the PFOSA dose Group animat 9R03- Liver PFOS] Liver PFOSA] O ver PFOSA PFOS Time Dose X X X ppm ppm eq ppm* Day 1 5 mg/kg 245 23.7 6.02 6.02 Day l 5 mg/kg 246 323 7.02 7.02 Day 1 5 mg/kg 247 363 6.24 634 Day l 5 mg/kg 248 21.2 6.66 6.66 Day i 5 mg/kg 249 27.8 8.81 8.81 Avg 28.2 6.95 6.95 SD 6.1 1.11 1.11 Range Min 21.2 6.02 6.02 Max 36.2 8.81 8.81 n Day 4 5 mg/kg 55 250 36.8 --S5- . 5 332 Day 4 5 mg/kg 251 32.6 3.47 3.47 Day 4 5 mg/kg 252 42.6 3.96 Day 4 5 mg/kg 253 36.9 3.45 ^45 Day 4 5 mg/kg Avg 254 38.3 37.4 * 4.11 3.70 * 4.11 3.70 SD 3.6 0.31 Range Min 32.6 3.45 0.31 3.45 Max 42.6 4.11 4.11 a 55 5 5 Day 29 5 mg/kg 255 20.3 0.09 0.09 Day 29 5 mg/kg 256 20.6 0.02 o!SI Day 29 5 mg/kg 257 22.0 0.10 O Day 29 5 mg/kg 258 26.2 0.14 0.14 Day 29 5 mg/kg Avg .............. 259 29.9 23.8 ** 0.30 0.13 * / ** 030 0.13 SD 4.1 0 .1 1 Range Min 20.3 0.02 0.11 Q.02 Max 29.9 0.30 0.30 n 55 5 5 1 Assuming a 1:1 ratio of PFOSArPFOS equivalents; Liver PFOSA PFOS equivalents =Liver PFOSA * =significantly different from day 1 values by a two tailed T-test (p<0.05) ** = significantly different from day 4 values by a two tailed T-test (p<0.05) PQL = practical quantitation limit in liver (PFOS = 30 ng/g; PFOSA 10ng) MDL = method detection limit in liver (PFOS = 15 ng/g; PFOSA = 5 ng/g) Page 13 o f 18 3MStrategic Toxicology ST39 T -7132.2 PFOSA PK study in rats Tab! 3 : Seram PFOSA am! m etabolites in the PFOSA Group . Time Day 1 Day 1 Day 1 Day I Day 1 Dose 5 mg/kg 5 mg/kg 5 mg/kg 5 mg/kg 5mg/kg Avg SD Range Day 4 Day 4 Day 4 Day 4 n 5 mg/kg 5 mg/kg 5 mg/kg 5 mg/kg animal # 9R 03- Sera [PFOS] XXX ------- JI5 ppm .9 24tT 10.8 237 $.4 245 6.7 249 7.3 8.2 1.8 Min 6.7 Max 10.8 55 250 7.8 251 7.5 252 11.3 253 8.6 Sera fPFOSA] ppm o? 3351 im 0.28 0.31 0.08 0.26 0.44 5 0.06 0.06 0.08 0.06 Sera PFOSA PFOS eq ppm1 05 333 0.28 0.31 0.08 026 0.44 5 0.06 0.06 0.08 0.06 Day 4 Day 29 Day 29 Day 29 Day 29 5 mg/kg Avg SD Range n 5 mg/kg 5 mg/kg 5 mg/kg 5 mg/kg 254 Min Mix 5 255 256 . 257 258 7.9 8.6 1.6 7.5 it.a 5 3.6 4.0 4.0 4.1 0.06 0.06 * 0.01 0.06 (JITS' --5 <LOD <LOD <LOD 0.06 0.06 0.01 0.06 aus 5 Day 29 5 mg/kg Avg SD Range n 259 Min Max 7.4 4.6 * / ** 1.5 3.59 7.36 5 0.0 0.0 5 5 1. Assuming a 1:1 ratio Of PFOSA :PFOS equivalents, Sera PFOSA PFOS equivalents =Sera PFOSA concentration * = significantly different from day 1 values by a two tailed T-test (p<0.05) ** = significantly different from day 4 values by a two tailed T-test (p<0.05) MDL = method detection limit (PFOS = 4.75 ng/ml; PFOSA = 2.89 ng/ml) LOD = limit of detection (PFOS = 1.74 nq/ml; PFOSA = 1.51 ng/ml) Page 14 o f 18 3M Strategic Toxicology ST39 T-7 32.2 PFOSA PK study in rats Table 4: Percent Dose Liver PFOS equivalents in PFOSA Group Time Dose Day 1 Day 1 Day 1 Day 1 Day 1 5 mg/kg 5 mg/kg 5 mg/kg 5 mg/kg 5 mg/kg Avg SD Range Day 4 Day 4 Day 4 Day 4 Day 4 n 5 mg/kg 5 mg/kg 5 mg/kg 5 mg/kg 5 mg/kg Avg SD Range Day 29 Day 29 Day 29 Day 29 Day 29 n 5 mg/kg 5 mg/kg 5 mg/kg 5 mg/kg 5 mg/kg Avg SD Range n anim al # 9R 03 -x x x 245 246 247 248 249 Min Max 5 250 251 252 253 254 Min Max 5 255 256 257 258 259 Min Max PFOS eq concentration in liver (p p m )' Total PFOS eq in whole liver (ug)* 29.7 309.1 39.3 401.1 42.4 462.6 27,9 281.4 36.6 391.7 35.2 369.2 6.2 73.4 27.9 281.4 42.4 462.6 55 40.3 455.6 36.1 422.0 46.6 563.4 40.4 456.0 42.4 41.1 496.2 478.6 * 3.8 54.2 36.1 422.0 4 6 .6 563.4 5.0 5.0 20.4 340.4 20.6 296.9 22.1 307.2 26.3 384.6 30.2 23.9 ft* 383.6 342.5 ft* 4.2 41.2 20.4 296.9 30.2 384.6 55 PFOS eq in % PFOS eq Residual % of PFOS in liver d o s e (u g )3 dosed found In PFOS In dose from residual liver 4 PFOS fn dose {%}* 1316.0 23.5 12.6 4.09% 1330.5 30.1 12.8 3.18% 1332.5 34.7 12.8 2.77% 1336.0 21.1 12.8 4.50% 1343.5 29.2 12.9 3.29% 1331.7 27.7 12.8 3,58% 10.1 5.5 0.1 0,73% 1316.0 21.1 12.6 2.77% 1343.5 34.7 12.9 4.56% 55 5 5 1333.Q 342 12.8 2.81% 1360.5 31,0 13.1 3.09% 1358.5 41.5 13.0 2.31% 1359.0 33.6 13.0 2.86% 1364.5 1358.1 36.4 35.3 ft 13.1 13.0 2.64% 2.74% 12.6 3.9 0,1 0.29% 1333.0 31.0 12.8 2.31% 1364.5 41.6 13.1 3.09% 5.0 5.0 5 5 1376.0 24.7 13.2 3.88% 1368.0 21.7 13.1 4.42% 1357.0 22.6 13.0 4.24% 1372.5 28.0 13.2 3.43% 1343.5 1363.4 28.6 25.1 ftft 12.9 13.1 3.36% 3.87% 13.2 3.1 0.1 0.47% 1343.5 21.7 12.9 3.36% 1376.0 28.6 13.2 4.42% 55 5 5 1. PFOS equivalents in liver (ppm) = liv er PFOS (ppm) + Liver PFOSA PFOS equivalents (ppm); 2. Total PFOS equivalents in whole liver (ug) = PFOS equivalent concentration in liver (ppm) * liver sight (g); 3, Assuming a 1:1 ratio of PFOSA:PFOS equivalents, PFOS equivalents in dose (ug) = Initial BW (g) * dose (mg/kg) = BW*5; 4. % PFOS eq dosed as PFOSA in liver =(PFOS equivalents in whole liver (ug)/ PFOS equivalents in dose)*100; 5. Residual PFOS in dose (ug) = dose` 0.96% * (5mg/kg*BW)0.0096; 6. % of PFOS in liver from residual PFOS in dose = (residual PFOS in dose/ total PFOS eq in Iiver+Vl4)* ! 00; * Significantly different from day 1 values by a two tailed T-test (p <0,05); ** Significantly different from day 4 values by a two tailed T-test (p<0.Q5); PQL = practical quantitation limit (PFOS - 30 ng/g; PFOSA 10ng) Page 15 o f 18 3M Strategie Toxicology ST39 T-7132.2 PFOSA PK study in rats Table 5: Percent Dose: Serum PFOS equivalents in PFOSA Group Tim e Day 1 Dose animal PFOS eq cone # 9R03- in Serum XXX (p p m )1 5 mg/kg 245 7,2 PFOS eq cone in liver (ppm) 29.7 Liver/se rum PFOS ratio (ppm /ppm ) 4.1 Total PFOS , Serum Eq in whole ' volume liver (ug) (m i)2 Total PFOS Eq in Serum (u g )3 309.3 8.3 60.0 Liver/ Serum PFOS eq % PFOS eq Residual % of PFOS in PFOS Eq in dose dosed found PFOS in serum from ratio * ( s )5 in serum* dose (u g f residual PFOS in dose 5.2 1316.0 4.6 12.6 21.1% Day 1 5 mg/kg 246 11.2 39.3 3.5 401.4 8.4 94.1 4.3 1330.5 7.1 12.8 13.6% Day 1 5 mg/kg 247 9.6 42.5 4.4 462.9 8.5 81.9 5.6 1332.5 6.1 12.8 15.6% Day 1 5 mg/kg 248 7.0 27.9 4.0 281.7 8.5 59.6 4.7 1336.0 4.5 12.8 21.5% Day 1 5 mg/kg 249 7.6 36.6 4.8 392.1 8.5 65.0 6.0 1343.5 4.8 12.9 19.8% Avg 8.5 35.2 4.2 369.5 8.5 72.1 S.2 1331.7 5.4 12.8 17.7% SD 1.8 6.2 0,5 73.4 0,1 15.3 0.7 10.1 1.1 0.1 3.5% Range Min 7.0 27.9 3.5 281.7 8.3 59.6 4.3 1316.0 4.5 12.6 13.6% Max 11.2 42.5 4.8 462.9 8.5 94.1 6.0 1343.5 7.1 12.9 21.5% N 5 5 5.00 5 55 5 55 55 5 Day 4 5 mg/kg 250 7.8 40.3 Day 4 5 mg/kg 251 7.5 36.1 5.1 455.8 9.2 4.8 422.2 9.5 72.5 71.7 6.3 1333.0 5.9 1360.5 5.4 12.8 5.3 13.1 17.6% 10*2% Day 4 5 mg/kg 252 11.4 46.6 4.1 563.6 9.5 108.2 5.2 1358.5 8.0 13.0 12.1% Day 4 5 mg/kg 253 8.7 40.4 4.7 456.1 9.4 81.6 5.6 1359.0 6.0 13.0 16.0% Day 4 5 mg/kg 254 8.0 42.4 5.3 496,4 9.3 74.2 6.7 1364.5 5.4 13.1 17.6% Avg 8.7 41.2 4.8 478.8 9.4 81.7 5.9 1355.1 6.0 13.0 15.9% SD 1.6 3.8 0.5 54.2 0.1 15.3 0.6 12.5 1.1 0.1 2.5% Range Min 7.5 36.1 4.1 422.2 9.2 71.7 5.2 1333.0 5.3 12.8 12.1% Max N5 11.4 5 48.6 5 5.3 563.6 9.5 108.2 5 55 5 6.7 1364.5 55 8.0 13.1 55 182% 5 Day 29 5 mg/kg 255 3.6 20.4 5.7 340.4 12,4 44.7 7.6 1376.0 3.2 13 2 29.6% Day 29 5 mg/kg 256 4.0 20.6 5.2 296.9 12.3 48.9 6.1 1368.0 3.6 13.1 26.9% Day 29 5 mg/kg 257 4.0 22.1 5.5 307.3 12.1 48.8 6.3 1357.0 3.6 13 0 26.7% Day 29 5 mg/kg 258 4.1 26.3 6.4 384.6 12.0 49.5 7.8 1372.5 3.6 13.2 28.6% Day 29 5 mg/kg Avg 259 7.4 4.6 * 30.2 23.9 ** 4.1 383.6 11.5 5.4 342.6 12.1 84.8 55.3 4.5 1343.5 6.5 1383.4 6.3 12.9 4.1 13.1 15.2% 23.7% SD 1.5 4.2 0.8 41.2 0.4 16.6 1.3 13.2 1.3 0.1 5.6% Range Min 3.6 20.4 4.1 296.9 11.5 44.7 4.5 1343.5 3.2 12.9 15.2% Max 7.4 3 0 2 6.4 384.6 12.4 84.8 7.8 1376.0 6.3 13.2 29.6% N 55 5 55 5 55 55 5 1, PFOS equivalents In sera (ppm) = sera PFOS (ppm) + sera PFOSA PFOS equivalents (ppm). 2, There are 32.3 m l Plasma per Kg of rat (9); 3. Total PFOS equivalents in sera (ug) = PFOS equivalent concentration in sera (ppm) *serum volume (ml); 4. Liver/ Serum total PFOS Eq ratio = total PFOS equivalents In whole liver (ug)/ total PFOS equivalents in serum (ug); S. Assuming a 1:1 ratio of PFOSA;PFOSA PFOS equivalents, PFOS equivalents in dose (ug) = Initial BW (g) *dose (mg/kg) * BW*5; 6.% PFOS equivalents dosed in serum (PFOS equivalents in sera (ug)/ PFOS equivalents In dose (ug)) *100; 5. Residual PFOS in dose (ug) = dose*0.96% = (5mg/kg*BW)0.0Q96; 6, % of PFOS in sera from residual PFOS in dose (residual PFOS in dose/ total PFOS eq lruera)*100; **Sign, different from dy 4 values by a two tailed T-test (p<0,05); MDL * method detection limit in sera: (PFOS - 4.75 ng/ml; PFOSA 2.89 ng/ml) Page 16 o f 18 3M Strategic Toxicology ST39 T-7132.2 PFOSA PK study in rats Table e - summary: % + SD of D ose or of PFOS Equivalents Dosed Detected In Liver & Sera Day 1 post dose day 4 post dose day 29 post dose % PFOSA dosed detected as PFOSA in: liver 5.4 + 0.9 sera 0.2 0.1 liver &sera 5.6 0.9 %PFOS Eaulvalents dosed detected as PFOS in: 3.2 0.3 0.0 0.0 3.2 0.3 0.1 + 0.1 0 .0+ 0.0 0.1 0.1 liver 22.0 5.2 32.3 3.7 25,2 +.3.0 sera 5,2 + 1.1 6.0+1.1 liver &sera 27.1 6.2 38.3 + 4.8 NA = not analyzed PFOS equivalents (ppm) = PFOS (ppm) + PFOSA PFOS equivalents (ppm) 4.1 + 1.2 29.3 + 3.8 3M Strategie Toxicology ST39 T-7132.2 PFOSA PK study in rats Table 7: Serum POAA iu th e PFOSA Grou 0. total % PUAA POAA in dosed animal Sera total POAA found as 9R03- POAA Serum in dose POAA in Time Dose XXX (ppm) (ug) (ug) sera Day 1 Day 1 Day 1 Day 1 5 mg/kg 5 mg/kg 5 mg/kg 5 mg/kg 245 0.11 0.90 3.29 27.3% 246 0.15 1.23 3.33 37.0% 247 0.13 1.09 3.33 32.8% 248 0.10 0.88 3.34 26.3% Day 1 5 mg/kg Avg 249 0.12 1.02 3.36 30.5% 0.12 1.02 3.33 30,8% SD 0.02 0.15 0.03 4.3% Range Min 0.10 0.88 3.29 26.3% Max 0.15 123 3.36 37.0% n 55555 Day 4 Day 4 Day 4 5 mg/kg 5 mg/kg 5 mg/kg 250 0.07 0.63 3.33 18.9% 251 0.07 0.64 3.40 18.9% 252 0.11 1.00 3.40 29.4% Day 4 5 rag/kg 253 0.10 0.95 3.40 28.0% Day 4 5 mg/kg 254 0.08 0.76 3.41 222% Avg SD Range Min 0.08 0.02 0.07 0.80 0.17 0.63 3.39 0.03 3.33 23.5% 5.0% 18.9% Max 0.11 1.00 3.41 29.4% n 55 555 Limit of detection (LOD): POAA 24.7 ng/ml NA: Not analyzed * based on work by Kris Hansen finding 2.5 ug/ml POAA in dosing solution 1There are 32.3 mL Plasma per Kg of rat.(13) Page 18 of 18 Laboratory Report Analytical Report of Data for PFOSA Pharmacokinetic Study in Rats (Sera and Liver) Laboratory Report No. FACT-TOX-145 (W2814) Requester Project No. T-7132.2 Testing Laboratory . 3M Environmental Technology & Safety Services 3M Environmental Laboratory Fluorine Analytical Chemistry Team (FACT) 2-3E-09 935 Bush Avenue, St. Paul, MN 55106 Laboratory Contact Kris Hansen, Ph.D. Bldg. 2-3E-09 P.O. Box 3331 St. Paul, MN 55133-3331 Phone: (651)778-6018 FAX: (651) 778-6176 Requester Andrew Seacat and Deanna Luebker 3M Company Toxicology Services 220-2E-02 St. Paul, MN l OF6 1 Introduction T h is study w as designed to prelim inarily assess the adsorption and m etabolism by the Sprague D aw ley tat o f the perfhiorooctanesulfonyl am ide (PFOSA Q F nSQ jN H j, CAS # 31506-32-8). T est anim als w ere dosed by oral gavage with 5 mg/kg o f PFOSA suspended in 2% TW EEN 80; control anim als w ere given 2% TW EEN 80 w ith no PFOSA. Subsets o fth e dosed group and the control group w ere sacrificed on day 1, day 4 , and day 29 post-dose. Sera and liver collected from the sacrificed anim als w ere sent to the Environm ental Lab and analyzed quantitatively for perflnorooctane sulfonate (PFOS, Q F n S O j', CAS # 2795-39-3), PFOSA, and perfluorooctanoate (POAA, C7F15CO2', CAS it 2991-51-7). PFOS and PFOSA were detected in the liv e n o f a ll dosed animals. PFOS lev els w ere highest in the day 4 group, but even liver from anim als sacrificed 29 days post dose w ere determ ined to contain high levels o f PFOS. PFO SA levels in the livers o f the dosed anim als were highest in the group sacrificed on day l ; on day 29, the average PFOSA level w as approxim ately 2.5 % o f the day 1 levels. PO A A w as not detected above the lim it o f quantitation in the livers o f dosed anim als. A s in the liver extracts, sera extracts collected 4 days post-dose evidenced the highest PFOS levels. Serum PFO SA levels decreased from day 1 to day 4 to day 29; on day 29, sera from four out o f fiv e anim als did not contain PFO SA above the lim it o f detection. PO A A w as detected in the sera o f anim als collected on day 1 and day 4. Screening studies o f the dose m aterial suggest that a sm all am ount o f PO A A w as present in the PFO SA dosing solution PFO SAB, (Q F iiSO jhN H , w as detected in the livers o f dosed anim als. T h is analyte w as also present in the solution used to dose the anim als. N o investigations o f PFOSAB in the sera w ere conducted The solution used to dose the test anim als w as analyzed to confirm the theoretical dose levels. The PFO SA concentration in the TW EEN 80 solution w as determ ined to be 1330 + /- 400 p g ta L . PFOS and PO A A were also identified in the dose solution. The concentration o f PFOS w as estim ated to be approxim ately 18.5 pg/m L; POAA levels are approximated at 2.5 pg/raL. PFOS and PO A A data w ere collected from a single analysis and should be considered to be o f screening quality only. A m ore thorough characterization o f the m aterial used to dose the anim als w as requested by 3M T oxicology and w as conducted by Fred D eroos prior to initiation o f the stud)'. R esults o f this m ore com prehensive characterization are available from the requestors. A lthough rigorous quality control m easures and 3M Environm ental Laboratory Standard Operating Procedures w ere follow ed, the acquisition o f this data w as not necessarily collected according to applicable G ood Laboratory Practices. N either the dose m aterial nor the analytical standards were given a certificate o f analysis; dose material w as characterized by NM R and LCM S and the analytical standards were characterized by NMR. The data presented here is not suitable for distribution to any governm ent agency in defense o f product suitability or safety. T his data is the highest quality data available at this tim e. 2 Sample Receipt On 10/6199,10/8/99, and 11/1/99 Deanna Luebker from 3M T oxicology Services shipped rat urine, feces, liver, and sera, sam ples to the FACT group in the 3M Environmental Laboratory, sam ples were received frozen on dry ice and were stored at -2 0 C. 3 ' Holding Times There is no holding tim e criteria associated w ith these sam ples for LC/ESM SM S analysis. 2 OF6 M ethods - A nalytical a n d Preparatory A n alytical m ethods E T S-8-4.1, Extraction o f Potassium Pcrfluorooctanesulfonale or Other Fluorochcm ical Com pounds from Serum for A nalysis U sing HPLC-EIearospray/M ass Spectrometry E T S -8-6.0, Extraction o f Potassium Perfluorooctanesulfonate or Other Fluorochcm ical Com pounds from L iver for A nalysis U sing H PLC-Elearospray/M ass Spectrometry E T S -8-5.1, A nalysis o f Potassium Perfluorooctanesulfonate or Other Fluorochem icals in Serum Extracts U sin g H PLC-Electrospray/M ass Spectrometry E T S -8-7.0, A nalysis o f Potassium Perfluorooctanesulfonate or Other Fluorochcm ical on L iver Extracts U sin g HPLC-Electrospray/M ass Spectrometry S am p le prep aration -H P L C /E SM SM S: ion -p airin g extraction A nalyte is extracted from sam ple matrix w ith ion pairing reagent [tetrabutyl am m onium hydrogen sulfate (T B A )] in a pH -controlled environm ent. T he cationic reagent selectively targets anionic fluorochem icals. O nce the anion-TBA pair is formed, the analyte is transferred into a non-polar organic solvent (m ethyl-iertbutyl ether), dried, and reconstituted in m ethanol for M S analysis. H P L C /E SM SM S In HPLC, an aliquot o f extract is injected and passed through a reverse phase liquid chrom atographic colu m a B ased on the affinity o f the analyte for the stationary phase in the colum n relative to the liquid m obile phase, the analyte is retained for a characteristic amount o f rime. For exam ple, in a standard solu tion PFOS m ay elute at 8.0 m inutes. R etention tim es betw een a standard PFOS solution and the analyte extracted from tissue in this analysis were m atched on the HPLC system to w ithin 1%. F ollow in g HPLC separation, ESM SM S provides a rapid and accurate m eans for analyzing a w ide range o f organic com pounds, including fluorochem icals. Electrospray, an ionization technique used prim arily for detection o f m olecular ions, is generally operated at relatively m ild temperatures. M olecules are ionized, and a primary ion, characteristic o f the analyte, is selected. This ion is bombarded w ith high-energy gas; subsequent collision s create sm aller secondary ionic fragm ents unique to the primary ion , w hich ate detected. For exam ple, for PFOS (Q F p S O /) analysis, ion 499 is selected as the characteristic primary ion. T his ion is fragm ented into other ion s such as 80 am u (corresponding to S O /), and 230 am u (C/FtSCV). Each o f these secondary fragm ents is detected and can be used to differentiate PFOS from other com pounds that m ight have the sam e characteristic 499 am u primary ion, but different chem ical com positions and secondary ion fragmentation patterns. 4 Analysis 4.1 Calibration Q uantitation o f the target analytes is based on linear regression analysis (w eighted 1/x) o f tw o extracted m atrix curves bracketing each group o f sam ples. Quantitation o f each analyte is based in the response o f on e or more sp ecific daughter ions using the m ultiple response-m onitoring m ode o f the instrument. A m id-level, extracted m atrix calibration check standard is analyzed every 5-10 sam ples to m onitor instrum ental drift. Calibration check standards are com pliant i f instrumental response is w ithin + /- 30% o f the expected value. 3 OF6 4.2 Blanks T w o extraction blanks, utilizing water as surrogate m atrix, are extracted w ith each batch o f sam ples. A dditionally, two sam ples o f blank m atrix (both liver and sera) ate extracted alon g w ith each batch o f sam ples and curves. Blanks are com pliant if no target analyte is detected above the lim it o f detection for a sp ecific analyte. In this study, all blanks were com pliant 4.3 Surrogates TetraTrydroperfluorooctanesulfonaic is used as a surrogate in this analysis. Surrogate response is m onitored to confirm gross instrumental M u re, If necessary. In the non-diluted sam ples, the surrogate response w as acceptable (+/-50% ) for a ll analyses. 4.4 Matrix Spikes D uplicate matrix spike analyses u tilizin g all target analytes w ere prepared and analyzed for on e control anim al. W ith one exception, PFO S recoveries were w ithin the acceptable range o f 70-130% . O ne liver m atrix spike showed a 66 % recoveiy for PFOS. AH PFO SA m atrix spike recoveries w ere acceptable for PFO SA A s POAA was not a target analyte in this analysis, no m atrix spikes w ere prepared. A lthough the recovery o f POAA from sera and liver has been verified for other studies, P O A A results should be considered screening quality only. O ne m atrix spike w as prepared for each o f the target analytes in the dose verification study. Spike recovery for PFO SA w as 130%, PFOS w as 115% and POAA w as 121% 4.5 Laboratory Control Samples Laboratory Control Sam ples are not a com ponent o f th is study. 4.6 Sample Related Comments. Other m atrices submitted w ith this study w ill be analyzed as needed upon w ritten request from the sponsors. In the event o f further analysis, an additional report w ill be generated D ose verification w as conducted by evaluating diluted aliquots o f the dose against an unextracted standard curve. Triplicate dilutions o f the TW EEN 80 dose solution were analyzed fo r determ ination o f PFO SA; a single dilution w as analyzed for determ ination o f PFOS and POAA. ''5 Data Sum m ary - ; T he table o f results detailing the sera analysis is available in Attachm ent A . R esults o f the liver analysis are presented in Attachm ent B. PFOS and PFO SA were detected in the livers o f all dosed anim als. PFO S levels w ere highest in the day 4 group, but even day 29 group anim als w ere determ ined to contain high levels o f PFO S. PFO SA lev els in the livers o f the dosed anim als were highest in the group sacrificed on day 1; on day 2 9 , the average PFO SA level w as approxim ately 2.5 % o f the day 1 levels. PO A A w as not detected above th e lim it o f quantitation in dosed anim als. A s in the liver extracts, sera extracts collected 4 days post-dose evidenced the h igh est PFO S levels. Serum PFO SA levels decreased from day 1 to day 4 to day 29; on day 29, sera from four out o f fiv e anim als did not contain PFO SA above the lim it o f detection. PO A A w as detected in the sera o f anim als collected on day 1 and day 4 . Screening studies o f the dose m aterial suggest that a sm all am ount o f PO A A w as present in the PFO SA dosing solution PFO SAB w as detected in the livers o f dosed anim als. T his analyte w as also present in the solution used to dose the anim als. N o investigations o f PFO SAB in the sera w ere conducted. 4 OF6 The solution used to dose the test anim als w as analyzed to confirm dose levels. T he PFO SA concentration in the TW EEN 80 solution w as determ ined to b e 1330 + /- 400 pg/m L. PFO S and PO A A w ere a lso identified in the d ose solu tion The concentration o f PFO S w as estim ated to be approxim ately 18.5 pg/m L; PO A A levels arc approxim ated at 2.5 pg/m L. PFOS and PO A A data w ere collected from a sin g le analysis and should be considered to be o f screening quality only. 6 D ata Quality Objectives and Data Integrity k vm m m m m N o circum stances existed during the present study that w ould have adversely affected the quality or integrity o f the data. T he follow ing data quality objectives w ere follow ed during the study; Linearity - The correlation coefficient (i* 2 ) o f the standard curve w as equal to or greater than 0.98 using 1/x w eighting L im its o f detection (defined as 'A the LOQ) - PFOS in sera is 4.88 n g / m L; PFOS in liver is 15.3 n g / g; PFO SA in sera is 2.47 n g / mL; PFO SA in liver is 6 .2 n g / g L im its o f quantitation (defined as the low est extracted standard accurate to w ithin 30% o f theoretical valu e) * PFOS in sera is 9.76 ng / mL; PFOS in liver is 30.7 n g / g; PFO SA in sera is 4.93 n g / mL; PFO SA in liver is 12.4 ng / g D uplication fiequency/acceptable precision < 30% Spike fiequency/acceptable recoveries - 70% to 130%; PFOS recovery w as 6 6 % for a sin gle matrix sp ik e in liver (see Section 4.4) U se o f confirmatory m ethods - no confirm atory m ethods were used Dem onstration o f sp ecificity -sp ecificity w as dem onstrated by chrom atographic retention tim e and m ass spectral characterization o f a single product ion G iven the parameters listed above, and assum ing spike recoveries form a suitable indication o f endogenous analyte recovery, data are quantitative to + /- 30% The validity o f this assum ption has not been verified by other techniques. 7 Attachm ents A ttachm ent A: T able o f results o f sera an alysis A ttachm ent B: T able o f resu lts o f liv er an alysis A ttachm ent C: Sam ple receipt A ttachm ent D: Screening results o f d ose verification A ttachm ent E: Extraction and analytical data 5 OF 6 S ign atu re* . . . A -__CLlp& fS ___________________________ ________________B l . o i ' f a _______________ L isa Q em en, Advanced Chem ist D ate ......( k - ---------------------------- - K ris H ansen, Ph.D ., Principal A nalytical Investigator _____________ W o y / 4 9 D ate 6 OF6 L ab oratory R ep ort 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 A Table ofResults - Sera Analysis Iip'f!*=3 2o : 2p :e i i II H i! i i 1'- !* ! [ ! 8 i *!f*<3V iiI ' _ Si ipil II? 3 S333 lisie Pili HUI lili! I?l?i!i!?i lili iliii m888s8?8RIUII m 23 iBUlSi8niSiB*i IIIII 3 Ii i! ES l !! IirSi?iiIfFIii SIlSflS5E !7 111 i i!i i l s p r r r f r g r s * ^ w * * V H-Xe<aisii li Il i i i i i i i i ? 33 t5 t V ii ii *f I SSB S il II B S i i o 3 i o i 1a i i H! * YSCW ' Rii r- x" S* o i o ; i o i a i s1* Ir 5? >X>X>Z >X >T :ss: 88858? 8 88o8>8p8 8o80o88 >z>>z 88z>z0z>z>88R II. i1**i oi i0s0s0H0s iiiii iii >zz>II z>z>ii r-* X z lis O SC z> 0? 0 z> o Z> z> i z> z> o z **>8 z w z 3 s a* 0 o i X z z S* z z o z0 > 1 > g 5 i Vm u5-8- -86P s S c E 3SSs o88a*888o s i i l i iiiii 5 H 8 8 S 0 a 88 00 Si ss R filli SISU0000 0 0 0 3ESSS iliii iiiii iiiii 33 13 ii ooii ii l I8 P i i i 3 3 8 5O i i m i = 5 oS i o ? 2 O1 5O i i Ifi 0 a B y LaboratoryReport 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 B Table ofResults - Liver Analysis U E 5 rnrm m I II l 38.fa 15 a.1 *R f l H SI II i f SI SU i* B iV i =s il Il r S-.i ?! X<X*X*T<BX3 S3 S 3 2 3 3 22888 28822 288 1 |5 mGMOKOt2OiiKOsUODK*ifOK iKOiKOftiOl l i H12 35 88 ll 8MmS8M5f 2M5i ?8uM3 8Hi5 3pS*mJ3ae!8gis3eugl 3eeje8BD53*a38OS4O83!tDS32a Dg58i 5g!$li a ACi l c'If \si i l 5"E;-sESi VM? B{P*wi l i l i 13 O [f 1 'illii' 1 I 1 !? sgg i t i l i gaslsagsgi SESSI c il5 d K S 2 ppp pp 89388 3 35 *p p p p P 88888 p r p p PP 85 88 88 1* h aKKg b b W CS SBSHHSHiA A t A i A l A i AAP A A i r e i Illii S3 33 33 AA 8 i i il *[ | 5| f | g E 23 3 ta S g fk i A %$ i .im tp H 1 1 S.5J J X mftr =s M o i O i / * Ai o o o h3 ili 32 ip i 3 1= f ! 1| S5 1 S5 iS 8 *S t 3 K i t i l i II s- s5tJK"p8*Stoap8*G*p8 p 8 p 2 S Si gp p 88 3 58 35 28 8 p p 88 pp 88 ih '* !r t 4 ft p J!l 1 p 2 a 5 a 2 o 5 * * =* 5 5 SS l l AAP AA li iil il 11 33 n A A fi II if si If i i" fl sO> M 3 b i o ** * i o i I 1 i l fij tttt lili .f 2 il S8 - eS_ - 1 o i o i T? o o 1 f=s?,s51 n O 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 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: 0 0 1 0 5 3 5 0 0 9 DATE RECEIVED: 1 0 /0 6 /1 9 9 9 DESC: PFOSA PK STUDY IN RATS TO X-145 CONTRACT L A B (S ): EXP COMP DATE: 1 2 /3 0 /1 9 9 9 DATE COMPLETED: PROJECT LEAD: KJ HANSEN PHONE NO: 6 5 1 -7 7 8 -6 0 1 8 3M FAX NO: 6 5 1 -7 7 8 -6 1 7 6 2 2 0 -2 E -0 2 ,7 -1374 SAMPLE DATE CODE DESCRIPTION RESULT MDL o r (95% C . I . ) 1 KJH-SPEC SPECIAL STUDY - KJH # # = UPDATED DATA 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 9RQ3233 9R03234 9R03245 9R03246 9R03247 9R03248 9R03249 DAY 2 DATE 10/6/99 Gen.MALE POST DOSE URINE ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 FECES ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 Chain of Custody Record 3M E n viron m en tal L aboratory Form 35176-PW O 3M Facility Cj V~iQ U /T jjc. ~ 7 b i Addiess 3M Pioject Trtte P P o S /h P /< 3M Facility Contact 09303 .T toM A ** 3M Requester . j rxoAnr^. U j d y - 3 ^ Project Lead ftorfjud S t L o J - 3M Project Nufltbt . Y - n r e a . a - i i / t e t s ~ r -TfSP.Q -tfw ' 3M Department Ntxnber Cy, State. Zip Code A r ' / i n m - L u c tM P ~ 3M Telephone Number ca a n Lab R e q u e st!ttn p la i*Jta m u cr ... 1 = I 2 2 L _________________________________________________ I Q 3 % i f Total Containers of Each Item BySampled jPunt) T V m WK. L u tb f r f ' Sampler Signature -. Contractor Data Number Containers of each Preservatives Q Samples Split See Attachment Comments J L 4 & /} Item # I l ' Sample YDescription (in1 i y i f U - f d S O nfj 2 rip " a a 3 D y f f h S f D o frrC 4 D y Z . >< /> r' 5 n ' j / P f S d S o L v t / '" 6 r i11 <v ^ C L - 7 t o f t e t f C t __________ Date Time Matrix in If) i/?yy L i n n C j / t l / O &J* IL r.t)C j m K (/? m I r r c S lO /L p fV L Z l ift/S p t m U X S ~ ( O f t cT b n \ zco r> ozZ 8XM z 8Z 8 G1 0 s - m o t r v i , S rw a f^ q n 7 // u ^ it 1 1 rm t* / ^ S n ylK <1 P f a. t* n n Cl>''r r D t ^ < 2 a S J 3 o - 3 - j h d J SrrynkjP K 8 9 10 ...............-------------------------------------------------- 1 -- 11 'Pfa f a 12 - ..... 13 ______________________ _______________ Item 1 // Relinquished By/Affiliatlon D m A nri U tib k fr Time Date ID h (M Shipped Via Received By/Afliliatlon / 'T & U h ! M M s M Time Date Y / j . ' y j r ^/--& / / 6 >r /*l f9 O .'gi.tat Accoirj.ji'y.-M ^ See Reverse Side For Instructions PFOSA PK STUDY IN RATS TOX-145 <LR #W 2B* DAY 3 DATE 10/7/99 Gen.MALE POST DOSE URINE ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 FECES ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 DAY 4 DATE 10/8/99 Gen.MALE POST DOSE URINE ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 FECES ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 LIVER ID# SERA ID# 9R03235 9R03235 9R03236 9R03236 9R03237 9R03237 9R03238 9R03238 9R03239 9R03250 9R03239 9R03250 9R03251 ' 9R03251 9R03252 9R03252 9R032S3 9R03254 g)9R 03254 PFOSA PK STUDY IN RATS TOX-145 . LR#W2814 D A Y 3 DATE 10/7/99 Gen. MALE POSTOOSE URINE ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 FECES ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R032S9 D A Y 4 DATE 10/8/99 Gen.MALE POSTOOSE URINE 10# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R032S7 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 9RQ3252 9R03252 9R03253 9R03254 g)9R03254 Chain of Custody Record 3M Environmental Laboratory 09600 3M Project Lead L u e b k it^ rTM111 - F6fm 35176 PW 3M Facility ( Odrunl'C 1 6 / Add'est / S9crJE - ^- City. Slate. 2<p Coo 3M Project Titta jN -p r^ / 3M Facility Contact Tiratnrto*-- 3M Telephone Number T- im T o y IM S 3W Profeti Number TT^-to-J. OolnriTuo'! 3M Ocyanment Number Lab R e quejvl empiate N..mcei --- pa i/ f Sampled By (Pimi) Contractor P tfx n /Y j. U ? b /c r ~ Sampler S*ntw* _ / Oate ( l 'cla u v / l Item ( I Sample Description l i n w ______ Date Time Matrix 1 T u /-? R > CJ D e , f j ILr . r i t , ,3/701 U n n f j 2 , , ' u i< n - F c c t S * / b / 1 / i p r A I c e / 3 0 / 1 " ' 4 t* ' f i ` " U r ,n iM L -fc c c s tln f -s ftc e ./. 5 D / -- Number Containers of each Preservative ft 2g n ozz 8N z 1 g 8 9x 10 ftp 1 \ \ p--/ j ZJ ---------- - ` t & r - w V h !t *- n ...... ------------------- 12 13 ~ = = ^ - -- - ......... .. -- 1 1,1 --1" ------ Item # Relinquished By/Affillation Time Oate Shipped Via Received By/AKlIlatlon Time Date / - Cp T X anra L u cb^ r / m s: /h a il u n r fif A CLbe^ / l / h H oo^rv J b i J i t (Id y iiia l A it .n 'i j.ji i , b .f i. j !, II c m ) U C 'Iw fa See Reverse Side For Instructions PFOSA PK STUDY IN RATS TOX-145 LR#W2814 DAY 29 DATE 11/2/99 Gen.MALE POST DOSE LIVER ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 SERA ID# 9R03240 9R03241 9R03242 9R03243 9R03244 9R03255 9R03256 9R03257 9R03258 9R03259 Chain of Custody Record 3M Environmental Laboratory Fom \ 35176 PWO 3M Facility CosyytMxj-cj ~7i>/ Address City. Stai. 2>p Coda 09305 3MRequenai 3MDAPiCojectAl*rdt G - ' 3M Project THI* P FdS K - 3M FaciWy Contaci ~PtC O t p o . in k & ts P K a r \n c K , { A 3M Talepnona NumOtf W- 7 - / 3 kd b X ^ r- tnYiH $P ^ p'J> *35 O 3M D o p j# w W Number la b R e q g e iv lempiei? Number uua&w Sampled 6y jPnntj ~yCcl*1/1&~ U 4 C & k zC r- S am p le /S ig n a tu re C orti actor Date Item * ( / Sample Description U J G L / L i Date Time Matrix 1 3 ~*J~ (/r->i 'r fr AVi/n/ <i /p M 2 P - r d r t f x s - `Z r t q / t ' q f r t f f r 3 y c c t s & ~ ic jv U / ( M t m i 4 Q /rfJ szu iw iii6 } r ft& 9 */ < 5 t<1o- l n u ^ U L ,< L n i* t* Number Containers of each Preservatives zco n aM X I l 6 7 8 9 10 ----- Z 3 Z 3 5 & =*- -7/ JFL d.J4 11 12 13 G Samples Split See Attachment | . Comments f v- *S K _S _ 5 ~ ---------"----- -- ' 111 ====" ------------ -------------------------_ i Item # Relinquished By/Afflllation Time Date Shipped Via ^Bqceived By/Affillation Time Date i- H D r n r * ^ U c b k > r /7 & l G j O i i & m . & x & a t < J C . O l .g - l jl I <' iim i'l u See Reverse Side For Inslruclions LaboratoryReport 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 ofDose Verification T0X I4J T ** IO- Dow C W m itiM Study Dale Analysed File Instrument TOAA Sample ID Twen dose-NA 70XH U/2/9* 110299 Soup 020199 D esetaae. (ppb) E ip re te d Dose (ppb) Ami f spike (ppb) Dmc MS (ne. (ppb) % Recovery D ese _____________ l \ m 20 4 29.48 VALUEl % ftecercry fMS O itis fC tlrs tlie e 121 11/2/99 nos Sample IO Twren doae*20ppb Dm * cmc. (ppb) C ip rtle d 0 *m (ppb) Ami ( spike (ppb) Pese MS c a a c (ppb) % Rccevery f Ds m ^ % Recovery f MS Date *( E itrs c tU a 36 9 2 0 0 20.7 601 . _ l y ) 115 J 1/199 Study Date Analyzed File# Instrument TOX145 10/29/99 102999a Soup 020199 PFOSA in 2%T w een 80, Sample TN-A-3046 File# 10299013 10299014 10299017 %Recovery of Dose Recovery of Dose amt (ppb) 132.64 265.27 134.31 268.62 132.83 265.65 Mean Standard Dev. %RSD 133.26 0.917 0.688 266.51 1.83 0.688 TOXUJ Titecrt IO- Dove Confiraxlio* Study Date Analyzed File * Injtfuinent POM S in p l i ID Tween dose*2ppb PFOS S an p lelD Tween do**>2ppb TOXI45 10/29/99 102999 Soup 020199 Dote cm (- (ppb) Expected Dea* (ppb) A n i of pike (ppb) Do** + MS rone, (p % Recovery of,Dos H Recovery ef M Date of C i t r t c l i i 6? 20 0 204 3 SI > __ 10/29/99 X De** cene, jppb) E tpetled Deic (ppb) A m e f ip ik t (ppb) Dote * MS cone, (p % Recovery oJ fip. % Recevery ef A) Dole of Extrac(ien 4U 2 QQ 201 6 40 / 207 * III? ) 10/29/99 7 " ------------------------------- PFOSA S aap lc ID Tween do*c*200ppb Doe CMC. (ppb| Expected Ooae (ppb) A m e i t p k i (ppb) D o 4 MS t n t . (p *h Recovery Recevery et M Dele ol Extraction Z . 3!___ "ij26565 200 100 385 42 -- ) ICV2W99 FACT: DATA REVIEW SUMMARY t-UKM One " / '/ / f i Data Analyst. f a c t s t u d y <. T o * -i< js M atnx/T im epoints: Sample Ust: o /Voce / i i i . . / , ) . S * j~ * h f Set-up A/ulysis Date/Analyst: d i f / n JA-i Instrument _____ JSs<71 Analyte: T&a a (<->* 0 Acceptable Linear Range LOQ: -- ____ R*2: 0^7/Z/ Extraction Blank: M * Matrix Blank: AM |Calibta*ion Checks: K - /S w > i - '/* J e m / d * A ^ MS/MSD: Data Status: Analyte: p F 3' C c H ^ ')Q > [Acceptable Linear Range: l i ) i LOQ. J L z iffk -- - R-2: ______ ~ ^ fo fp p h . Extracted Blank: M a Matrix Blank: A/fl Calibration Checks: & K ' /5 ^ ^ -// M S / M S D : _______ Data Status: (? * / Analyte: 'CM3;Z F Acceptable Linear Range: LOQ: h . / 0 ,, l T f" Extracted Blank:___/__I IT2: O i Z l f Matrix Blank: a/A Calibration Checks: -- 2 & / j , e d t J j c L /o % MS/MSD:_____________ ___ __________________ D ata Satus: Data Review Sign-Off Analyst Review Nimc /Otie: //'A d i i - Technical Review Name/Date:____ Quality Assurance Review Name / Date:______________ Data Entry:. Comments I Justifications: TU ZS/ kje.** . a --e / __ -/rj*- 4 L t cu.v-4/er /*- O r d i y ' */> _______ L>*v ~Ll I t ' ji u r /w k 3 ba-Xt-cJ o / / rug - j s^c<va/rc<; /^ J * '* ' <9 a . ~ d 7^ M Ca.ftj''My' ics*-S K ^ -tc < c/ dh h 4u A cj/^ # 7 - 3>a 'V o r/y f O: 7 5 2 rt^l, j f u d * jL*r<__ d f p i ^ j 4 U - lu jL r __f * V<d**s n i f e s s d d ~ o -. U . 4u^ f^ A fartir^rv/H ./s . kM s u d n u d 4L L JL&UXiV C&/LC $ j -c C *t ^k wr yj ia(m! k * ~fc_ f k t o t f g / k s ___ f-?J f fJ i_*---J dr /a- o r r fr ,- 4 c /U ., '>u d \ ?Vs f L - d i ^ - /.-,? J .^ o- FACT: DATA REVIEW SUMMARY FORM Oata Analyse: -A4* FACT Study a: T`/S ' Malnx/TimepoinU: ~7uxt.iL. ffo ofc-f Sample List: io 7 t f 1 a. .a*xJt+.L- Set-up Analysis Date/Analyst: Instrument: Analyte: J s phihi 7 / ) Accesttble linear Ranne: A/A LOO: AM R"2: Att Extraction Blank: a M Matrix Blank: AM Calibration Checks: f/A MS/MSD: Data Status: Oita Review Sipt-Off Analyst Review Name I Daw: /, /w /tf .......... t o H /I/J 3 , Quality Assurance Review Name / Date:___________ Data Entry: _ Comments/ Justifications: ,________________________ <3>___________.erg '/ / ___ L u *. -- h.n pe> I f M - s T C &Mfi tlf i* * 1m J fhi t B i t s . W Z s-rp ^ - 7 * * n/* > if a k * f t c 4 t / A<_ 7 ^ jk s - " A /A t Otaai/c F<tf ><*// a jIu u c J ' ~fL* S d * j> lr yu H . "'fytn/f+* UCK a s L j L as. 5 f* /a A > / . td j 4 i - JA y ' 'J 'yLL. * ehrir-oN><oho^jirr-` r*r>-4f' in^tOrtmn 0 0 4 o 4 lonnn Si i i i i i i i i s u u iSiill J. i Om r( wn n ^ . OMHOOOr 222 SS ? 2 ? ? * *r f- f- i-> r- r vSnuiwj nuf mTiCru vmww } im i i! 8 8 1 11I H i3 I i1 b 'LM*i. a_ Ub* o* 0o*a*m*1 0oro*04f4 s3i .r..i..s... ,:t i S sL V if wES! ! 3" *2 SsS? S ii i i l l l i .a a o t oa aa9aSa 9 " I | S Bo*i sa** O*sM^ j " Si" 47TO5 <SI*Sovs 's Be * > I7' H^ I! Hf un !! *> tss> i. i -9^3 a a aci lillllsls si l > JM 33% J o o o o o o o o ! 2 S 2 2 S SS liiiliiiiiiiiiiliilliiiiiii ! e , * f*, ' * * * * * i * * , *'o oooooooooooooooooooooooo i : I a I t9ffi1tt I ? >o o o o c **** '*- * >< ,. k<M^ m S ooooooooooooof i S2>.oIpS'*'<,3 --'** " OOQOOOOOOQOOOOOilO 3000&0000 " ; , r - *` -u'-w r Ot nOOtOAOOOOlB/io UO tiTivq'Otifi c V f l tn jtr i i a tr V tr * it.. 0 0 0 0 `^' ^' V> < M < w iiHI** T *D5.O*I *i' *a s* aSs: 099 S* w O1 -S o 0*0 o i "'S x> <y *o ' *51 0o**O'l, O-r,t * V > W>1 -J U !.. J - *>*9 9 ss? f* : WUIMHIPUwUiH 'OlPOOU'otMJ 00 0 00$ s ssoaou ttr -ero>i w o > ''i* i !4 8 3 * o a SOls lO 5o ti s \ \i l -uw* oCo6ooowooMooweha uw-W>0 ;s4t g g g m m m a m p g g g s m ? ;! > U IP O W U O I/ < ,H V 'U |l > 5 SSllSSSiisSSSS s s 1 3 ? e & I n e Method Report Method t i l : Lest modi f t e d : C om pound P rin te d : C:\MASSLYNXiaoup020199.praiHethD8\102999a.axib Mon MOV 01 0 < 2 l : 4 0 19 . 1 : POAA ( C h i : Mon Nov 01 09:34:09 1999 Compound Mease: In te rn a l R ef.: Q uantify Tree: Cone, o f Standards: User RF V alue; User Peak F acto r: in t e g r a t e Window F acto r: Chromatogram mass window: POAA (Chi: {None} TIC Cone. A 1.000040, 1 . 000000 2.000 1.00000a O isebled R eten tio n Time <nuns 1: R elative Retention Tine: *7 R eference: Time Window t a i n s ) ; Peak S e le c tio n : 7.171. 0.000. (Monel 0.312 enabled D isab le d Nearest Response Type: Response-. E x ternal Areas Polynomial Type: Point of O rigin; F i t Weighting: Axis T ransform ation: Linear Exclude 1/X None U nits: Peak - to~pak am plitude: 90 Smooching: Window s iz e (scan s): Number o f smooths: Smoothing method: Enabled 1 Join valley threshold: Reduce peak t a i l i n g : Raise b a s e lin e maximum: 10.00 20 0 .0 0 5.00 Craw v e r t i c a l th re sh o ld : D etect shoulders: Shoulder threshold: 90.00 D isable d 10.00 R elative height: Absolute height: R elative area: Absolute area: 1.50, 0 .0 0 . 2 .4 0 . 0.00. D isable d D isabled D isabled O ia a b le d I Peg* Method Report Method f i l e : Lest ao d itied C o n fo u n d . P rinted: C: \MASSLYNX\soupO20I f 9.pro\HethJDI\102999a.mdb Mon Nov 01 0 6 :2 1 :4 0 1999 2 : PrOS ( C h i' Mon Nov 01 07:36:09 1999 Compound Heme: Incernsl R ef.: O uantify Trace: Cone- of S tandards: Uaer RP Value: User Peek f a c t o r : I n te g r a te Window F a c to r: Chromatogram u i i window: PFOS ICh2) (None] TIC Cone. B 1.000000. 1.000000 2.000 l.OOOODa D isab le d R eten tio n Time (suns; : R e la tiv e R eten tio n Time: R7 R eference: Tine Window ;m n s ; : Peak S e le c tio n : 7 .(3 4 . 0-000. (None] 0.3(5 Enabled D isab le d N earest Rcsponee Type: Response: External Areas Polynomial Type: Point of o rig in : P ic Weighting-. Axis T ran sfo rm atio n . Linear Exc lu d e 1/X None U nits- Peak-to-peaa am plitude 68 Smootning. Window s u e ( s c a n s . Number of smooths: Smooching method: Enabled 1 Join valley threshold: Reduce peak t a i l i n g ; R aise b a s e lin e maximum: Draw v e r t i c a l th re sh o ld : Detect shoulders: Shoulder th re sh o ld : R e la tiv e height.Absrluce height: R elative area: Absolute area 30.00 2 0 0 .0C 5.00 90.00 D isabled 30-00 l.S C , 0 00. 2.00. 0.00. (Disabled D isable d D isab led D isab led Pag TQQuXan14tiSf-ycc*aalibtoradtieon cMopaofirrtaacioa Cor rOJU. rfOS. 6 bOAA- at. 10/29/99 iat Compound 1 name: POAA (Ch1) (Coefficient of Determination: 0.997121 Calibration curve: 10.0347 * x + 5.23213 #0 l 0201 11 01Coup * : Q u a n t i t a t e d a d p r i n t e d iry l a a on / / Q uastlfy C a lib ra tio n *pore TOXllS-tw*n ao do* co stiv iM X io a i o r PQJUk, r r o , * KUA- a x e . 1 0 /2 4 /9 * 1** Compound 2 name: PFO S (Ch2) Coefficient of Determination: 0.996935 Calibration curve: 86 .057 7 ' x + 68.0228 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None 3 ` : Soup 0 2 0 19 9 : O u a a t ie a c * and p r l a c d toy la * o a 1 1 / 0 1 /9 9 TQOuXaai4e9if'tywCanlib0radtoio*n* oRoepoofritnutloo for KU, PF04, 4 fOAA- **t. 10/29/99 4a* ICompound 3 name: PFO SA (Ch3) Coefficient of Determination: 0.997261 (Calibration curve: 27 2.18 9 * x + 203.159 iResponse type: External Std, Area iCurve type: Linear. Origin: Exclude. Weighting: 1/x, Axis trans: None Q uantify C a lib ra tio n JU port TOX14S-c*Ma 0 d o M c o n f ir m a t i o n f o r r o u . rrot. ft 0 * 4 - M t . 10/29/99 l u iCompound 4 name: IS (Ch4) Response Factor: 2904.16 Response type: External Std, Area Curve type: RF ; 4.49e3-1, i! i 4 Soup 020199: Q u a n tita te d an d p r i n t e d toy ta a oo 11/01/91 Laboratory Report Analytical Report of Data for PFOSA Pharmacokinetic Study in Rats (Sera and Liver) Laboratory Report No. FACT-TOX-145 (W2814) Requester Project No. T-7132.2 Attachment E Extraction and Analytical Data Extraction Worksheet ETS-8-6.0 Study T U X - /HJ~---------- Surrogate Std FC Mix FC Mix FC Mix Comments Verified By Matnx'^a.f, L iV i r ______ Approx, ppm approx.0.5 ppm approx.5 ppm approx.50 ppm Box # _ a x _ ii f i ___ Actual ppm actual ppm actual ppm actual ppm W K /D av A ^ 1 X4 #<Noflv-il-ll #1`>o&.-V72 # 9 * o fit-v )-/ t l i o s - 1 1 DateSpiked/Analyst >n-i R8L1039.250op6-CCV-l 1-Mo* 5 uL 9RQ3230M.Oy1.Controt-2SOpp6>MSmi1 5uL t o , ( f y s c ~ ,0-, !??/.'s ~ _ / O i l - W / j * - ' 10 uL - K>*3- - 10 uL - ' ftj A 9R0323SM.Oy4.Control.250po6'MS/Ol2 5 uL - 10 uL - R0I1O139-H2Ottk-11&12 5uL - - - RBL10139-vef Wk-11412 5 uL - - R0L1O139-Spot>*11&12 5 uL 2 uL RBL10139-I0ppb-11T2 5 uL 4 uL RBU0139-2Soob-t1&12 5 uL 10 uL - - RBL10l39-50pob-11412 5 uL 20 UL - - RBU0139-I00pp0*1l4l2 5 uL 40 uL - - RBLI0139-250ppfr-tl &12 5 uL - 10 uL - RBLtOl39-560pob-11&12 5uL . 20 uL - ( S t- R8UD139-750pp0-11412 ' R8L10139-l000ppt>-1l4l2 9R0323M.Dy1.Control 9R03231M.Dy1.Control 9R03232M.Dy1.Control 9R03233M.Dyl.Control 5 uL - 30 uL - 5 uL - - 4 uL 5 uL - - - 5uL - - - 5 uL - - - 5 uL - - - 1 ^1 SrtL. to h -, f r t 1 __ AllA 9R03234M.Dy1 .Control SuL - - - 9R03245M.Dy1.5mg/kg 5uL - - - 9R03246M.Dy t .5mg/kg SuL - - - 9R03247M.Dy1.5mg/kg 5 uL - - - 9RO3240M.Oyt .5mg/kg 5uL - - - 9R03249M. DyT.5mg/kg 5 uL - - - 9R03235M. Dy4.Control 5 uL - - - 9R03236M.Oy4.Control 5 uL - - - 9RQ3237M.Dy4.Control 5 uL - - - 9R0323flM.Dy4.Contrai 5 uL - - - 4' Blank - Ttaliti', 1 L -lv o v - Std# W o n , a - s ' amount * 1 - 0 ml 0 ./ ( , 1 g/ml Liver Extraction Method ETS-8-6.0 Data & Initials Vortex 15 Sec. Pipette Malnx, spike wrth appropriate surrogate or FC-Mix Volume___/_t-7r___rnl Pipette 1 ml of O.S M TBA. pH 10. pH=M2-- J & ^ l & = - ... Sd.' Pipette 2 ml of 0-25 M Na?CCV0.25 M NaHCOj buffer S tO VwiO - `V -Q j Ulu- Dispense 5 ml o< methyt-l-butyl ether Shake 20 min TN-A--yVv Shaker speed: 3t*-> E Centrifuge 20-25 min. Centrifuge speed: Remove a 4 ml aliquat of organic layer Put on Nitrogen Evaporator to dryness temperature: BnomJfiDL Add methanol Vortex 30 sec. Volume / <3 ml I , p--- TI N---A.^^-^alQrT--l--STTtrTBOB to-n -1 y /w Filter using a 3cc B-D syringe with a 0.2 urn filter into an autosampler vial 3 f t u - / ' 3 ' - n t o ( i c o o r p b "/ i >u >ojo a t d RT ^ j, Clr ^ Cri,^ o^t o \ 0 O O ^ Tf&yr-h M#wt eowt-* 10-/3* 10/12/99 Draft Attachment A ETS-8-6.0 Extraction of PFOS from Liver Form Cometetion j / Verified By tify Extraction W orksheet ETS-8-6.0 10/12/99 Draft Attachment A ETS-8-6.0 Extraction of PFOS from Liver Form Coi Verified Sample Weights/ Volumes P re p D ateli)', lu-12-99 A nalyst(s): SEE Sam ple M atrix: Rat Liver .M ethod/Revision: ETS-8-6.0 T arget A nalyte(s): PFOS. PFOSA Sam ple ID 9R03230M ,Dy I.Comrol 9 R 0 3 2 3 1M .D yl .Control 9R03232M .Dyl.Control 9R03233M .Dyl,Control 9R032J4M -Dyl.Control 9R03245M .Dyl,5m g/kg 9R03 246M ,Dy t .Smg/kg 9R03247M JDyI.5mg/lcg 9R03248M ,DyJ,5mg/kg 9R03249M .DyI.5m g/kg 9R0323iM .D y 4.Control 9R 03236M ,D y4.C ontrol 9R03237M .D y4,C ontrol 9R 03238M ,D y4.C ontrol 9R03239M ,Dy4Xontrol 9R 03250M ,D y4.5m *ficg 9R 0 3 2 5 1M .D y4.5m g/kg 9R 03252M .D y4.5m g/kg 9R03253M J3y4.3m g/kg 9R03254M .Dy4.Smg/kg . ____ Initial W eight gram s t.o irt / . OO0o 0.9978 / /il i-o n i /.0 O 7 V /.a/or l.olO l a. t i l l i . eotq 1. ooi.<4 a.ttov Study N um ber: TOX-145 Equipm ent N um ber: 0222*0900 F inal Solvent & T N N u m b er: M cOH / TN-A-2945 M atrix B iank/ldentifier: Rabbit Liver Box: 99-200 Hom ogcntxed By: V erified By: Com m ents /O/iJ/ff-.I c s /Jl a ____________ U s e d f o r M S / D 11 ___________ W i t __________________ ______________ i ____________ ___________ a ____________ M u t 1o fr k ftf^ __ Tn ) / n _ _ _ ____ U s e d fo r M S /D 12 (V /A A Oort, /. UOi Vl.eo-xl o -m i - o j i n _______ S' ? ____ 4 .. ............... ..................... " f? *-c-- ' Sum m ary of m ethod: Notes: Review Date. RU1Q139 Form A pproved by/D ate:___________________________ Form C o m p letio n o , / /M Verified B yrjd ttlsjQ jlljffi ionPwStmJardCurvaa-Tiam* Prrp Uali| AM<|lCfl: wewi : Tarfrt AwtfiNa): Bal NaaWr: una*' .SITE R.K Ll*r ETS--< f^Nii w .:oo Swily AeatWr. T0X-U5 FgaipaMatNMter 0222-0900 Fina Sa**M<* TT* N n k * r MeaHTN.A-Xras ftlaafc TitMWI4Mificr: Hibto rC M U S M A fftrat.O S O O p pm : FC MU SU A p p n t. SQUfpm; FC Mi* S u l A r r v - SOOppm: S rr |M Sed Appre. 100 ppm: < *K tb ~ i7 -2 -W JO ) *a0U ' t ) - l l A aw l Canceraratwa of SuvUaM 0>* FC Mut fFOS rroSA FFOSCA SU Cae SU Cae SU Cae *>crmL *i"L 0 5000 0 5000 0 5003 0 3050 0 4997 0 4997 05000 0 5050 0 4997 05000 0 5050 0 4497 0 5000 0 5050 04997 3000 5 005 4 997 5000 5 005 4 997 5 000 5.003 4*97 50 00 5005 49 97 PFOSAA SU Cae *<- _ 04999 04999 04499 04999 04999 4*99 4 999 4999 49 99 Nh 4tirariaiAal(hnty{() Mrcar*: fml *!*daa(nlHwwna: C tfQSC-Ott SU Cora. n 0 5005 OSOOS Q 50QS 0 5005 0 5005 5 005 3005 3003 5005 MSM SUConc w ArL 0 5010 0 5010 soto 0 5010 05010 5 010 3010 soto 30(0 A# A t Spikod mL 0002 0004 ooto 0020 0 040 0010 0.020 0 030 0.004 0143 I 000 A0 Ooraty 01*3 0 163 0163 0163 0 163 0143 0 143 0.143 0.143 C w a M n m ra rfS ini< ndi <n Oa ampia ira FFOS FFOSA FFOSCA SUConc SU Cae SUConc rt 6 13 6 14 6 13 12.3 (2 4 12 3 10 7 31 0 10 7 613 62 0 61J 131 124 123 307 JO? 307 613 614 13 920 021 920 122? 1221 1226 FFOSAA SUConc yi 13 123 30 7 41 1 123 307 13 920 1227 CaicvUtad Concanmion o f SlaiUarda ui Uc 10 L final vivera voiumt FFOS Final Cora FFOSA Final Cae FFOSCA Final Conc FFOSAA Fan! Cara nifmL n*/n\L rts/mL 100 1 00 1.00 100 200 2 02 200 200 300 5 05 500 300 10 0 10 l (0.0 100 30 0 20 2 200 200 500 50 1 500 50.0 100 100 100 100 150 150 150 ISO 200 200 200 200 KFOSC-OH SUConc rt 14 I2J 10? 1 4 123 307 14 921 1221 . __ E4FOSOOU Final Cora. tal. 100 200 SOI 100 200 50 1 100 150 200 SU Cara. y t AIS 12.3 JO? 61.5 123 JO? *15 922 1229 S anipw SUConc. mUL 100 S en atM Final Cora ______9 l _____ 1077 A4 A ntS pM mL 0003 MAM SU Cae. taL 100 200 301 100 200 50 J 100 1 200 iam pna SU Cora. ymL 100 SafW fiit FmUCora _____ _________ 502 AJI AmtSfwkarf nL 005 Sampie um! for M&WSO 9J103230ML Dyl Concrol MS7MSD cale. le mam liuual W m ) 0 996 FFOS FFOSA FFOSCA Final Conc. Final Cora. F m l Conc "Vi F i n 301 301 301 30) 301 301 FFOSAA Final Cara. V i 101 301 Iniri VofctfMmL)- 500 CiFOSC-OH MSM Vinal Cae. SU Cara y ' y 301 302 101 302 Apprra. SU Cora.. 5.00 uf/ml. Am'cSpUraKnL) Donan? 0.010 0144 Samplc uaad (ot MS/MSD 032J0M. P yl Control MS/MSD cac in aol<m Imial Wt (S) 0994 FFOS FFOSA FFOSCA Final Cene Final Cae Final Cae *V i i 500 50 1 500 500 50 1 500 Samplc vU fot MS-MSD 9R03235M. Dv4. cnrarol MS/MSD cale. In m a n Imm W tt ) 1 001 FFOS FFOSA FFOSCA Final Cae Final Conc Fmai Cae y* *F y* 301 301 301 J0I 301 301 Sampte uaed for MSMSO 0323SM. Dr4. v-envol .MS/MSD cale U oivcm Iranal Wi i<| 001 FFOS FFOSA FFOSCA Final Core Final Conc Final Cara _____ "y 500 30 0 ____ "-* 50 1 50 i "FS 500 500 FFOSAA Final Cae n#t 300 500 FFOSAA Final Cora y* MI MI FFOSAA Final Conc "y* 500 500 Jmual Volante <LV 5 00 EFOS-OH MSM FmalCone SU Cae ys "Fl 30) 301 50 1 50 Appeo*. SU Conc SOOua/mL AmtSp*a6<*il.) Fmal Val. 1 0010 1000 < ' i lwal VekimalniLh 5 00 CtfOSL-OH MSM Final Conc SU Cara "FS 1 301 102 101 302 Appre*. SU Cara. 500 uft/aU. A1 Spifcod (m t) Donan? 0010 0167 Intiial VolumelmU Cj FOSE-OH Final Cora y* 50 i SO 1 soo MAM SU Cara VI 50 1 50 1 Apprex SU Cae SOOmfatL Ainl SpUod (mi.) r U Val 0 010 1 000 ion Fax SU Esm eran Sha 1 11 ? | AJI Va i I I I I I I I 1 DILUTIONS SUMMARY SHEET Study: T O X -045 D ilution D ate/A nalyst: M C H 10/18/99 j m B ox#: 99-200 -io lith * sa m p le n u m b e r o r d escrp ilio n 9 R 0 3 2_3 7 M , D ay 4 , C o n tro l 9R032J5M . Day I, 5 mg/kg 9R03246M , Day I, 5 mg/kg 9R03247M . D ay I. 5 mg/kg 9R03248M . Day I. 5 mg/kg 9R03249M . Day t , J m g/kg 9 R 0 3 2 5 IM .D a y 4 , 3 mg/kg 9R03252M , Day 4, 3 m g/kg 9R03253M , D ay 4 ,5 m g/kg 9R03254M . D ay 4, 3 mg/kg 1: 10 0 D I00 D I00 D I00 D I00 D I00 D IO O D I00 D IO O D IO O D IO O l: I; I: S' ' -X Solvenf/TN Number: j l ^ O H E xtraction D ate/A nalyst: SEE , 10/13/99 M atrix/T im epoint: Rat Liver /^U/t<r fl,T D IL U T IO N S l: I : 1: C om m ents V erified By X' P o w t / H i m id u f a n r o /ft ^- 10 (1 2 (1 7 / fU /^ k iilitl- ID j l r / m 1 J j \/ , fn M - Hy h r ia s . Notes: D100=10 uL J*mple + 990 uL . \ Form Completion Verified By: \o-i v- ^ Extraction Worksheet ETS-8-4.1 Extraction W orksheet ETS-8-4.1 Sludv# "p-,. 1Hr Matrix " n.1 Surrogate Std FC Mix FC Mix FC Mix I Comments I Verified By I Approx, ppm approx.0.5 ppm approx.5 ppm approx.50 ppm Box # 9 d J\ ^ Actual ppm actual ppm actual ppm actual ppm VA/K/Dav 1 >M #9<nri.ii-il # 9ric it. t # licit. yvi 33 DateSpiked/Analyst lO II-V t/S c .'' tu - ll n / A c - ' ir RBS10199-2500P6-CCV-TM lo4 5 ul & RTS10199-250ppb-MS/D-11 RTS10199-Serum Blank-11&12 5 uL 5 uL - - 5uL ij 5uL ! l ___ RBS10199-H2O blk-11412 RBS10199-Serum blk-11412 RBS10199-5ppb-11412 RBS10199-10ppb-11S12 RBS10199-25ppb-11S12 5 UL 5 uL 5 uL 5 uL 5 uL IOuL 20 u l 5ul * - i RBS10199-50ppb-11412 RBS10199-100ppb-11412 RBS10199-250ppb-11412 RBS 10199-500ppb-11412 RBS10199-750ppb-11412 RBS10199-1000ppb-11412 9R03230M.Dy1,Control 9R03231M,0y 1.Control 9R03232M,Dy1 .Control 5 ut 5 uL 5 uL 5uL 5 uL 5uL 5 uL 5 uL 5 uL - 10 uL - - 20 uL - - - 5 uL - - 10 uL - - 15 uL * * 20 uL -* *- ' -- - . i 9R03233M,Dy1.Control 5 uL - * !i UtM o}mJ4 9R03234M.Dy1.Control 5 uL * - - rW/F ` 9R03245M,Dy1,5mg/kg 5 uL ' - 9R03246M.Dy1.5mg/kg 5 uL - - 9RQ3247M.Dy1.5mg/kg 5 uL - - * 9R03248M,Dy1 ,Smg/kg 5 UL - - - 1 9R03249M,Dy1,5mg/kg 5 uL - - ' 9R03235M ,Dy4 .Control 5 uL - - 9RQ3236M.Dy4.Control 5 uL - - - 9R03237M.Oy4,Control 5 uL - - - 9R03238M,Dy4,Cootrol 5 uL Bl ank' S, V Std# q<tck,a-3h lSenjmxtraction Method e t s-8-4.1 * amount = l O * ammmm..... J ____ Date 4 Initials LZ (Vortex 15 Sec. Pipette Matrix, spike with appropriate surrogate orFC-Mix Volume ______ _________________l*s==t VO ml 1 Pipette 1 ml of 0.5 MTBA, pH 10. pH= io- Kyi Pipette 2 ml of 0.25 M Na,CO,/0.25 M NaHCOj buffer Std. # M90C. Llk_________ L Std. # 9 QOft. -N- P. I Dispense 5 ml of methyM-butyl ether TN-A- jdW v, _ Shake 20 min Shaker speed: 3 0 0 Centrifuge 20-25 min. Centrifuge speed: 3 ) lIlirlD IQl ? -I . \y IVI* /u/K . |Remove a 4 ml aiiquat of organic layer (Put on Nitrogen Evaporator to dryness (Add methanol Volume 1O (vortex 30 sec. Temperature: Room Temp TN-A- | w m m 1 m m arni t i il" Filter using a 3cc B-D syringe with a 0.2 um filter into an autosampler vial .. [r \'(ItiK ffli& Ei (G. io f[U TK*. - * '' 9--- ^ c/*c W r< a W -- n '" /i-- 10/12/99 Draft Attachment A ETS-8-4.1 Extraction of PFOS from Serum Form Completion , / Verified Bv H I M Extraction W orksheet ETS-8-4.1 Study Urr ;a W V Matrix Tipi Box# 4n WK/nav a . 1* V Oate'Spiked/Analyst 9R03239M.Dy4.Control 9R032SOM.Dy4.5mg/Vg 9R03251M.Dy4.5mg/kg 9R03252M.Dy4.5mg/Vg 9R03253M.Dy4.5mg/Vg 9R03254M.Dy4,5mg/Vg . - - - ------------------: Surrogate Std Approx, ppm Actual ppm nH '/oit-iJ-n i<)-/ 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL FC Mix FC Mix FC Mix approx.0.5 ppm approx.5 ppm approx.50 ppm actual ppm actual ppm actual ppm # ,iA tv r - - :___ _Z - -y Comments Verified By N rt- ..Nr/,fi____ / ______ ' - y V / - k' -S ' .. / - * - - /- X: -- ' .. B l a n k s . V r , _____ Std# <?<?oC,73 Serum Extraction Method ETS-fl-4.1 amount * 1 ,0 ml____ Date & Initials Vortex 15 Sec. /r)-/y- Pipette Matrix, spike with appropriate surrogate or FC-Mix Volume. J _ 0 __ . ml Pipette 1 ml of 0.5 MTBA, pH 10. pH=_iu__ at/f- r r / ^ _ Pipette 2 ml of 0.25 MNajCCy0.25 M NaHCO, buffer Std # ly p & w j /fa_________ si.s t d . # j ^ , - ty Dispense 5 ml of methyl-t-butyl ether TN-A- Jtr/C* Shake 20 min Shaker speed y Centrifuge 20-25 min. Centrifuge speed: ICDO Remove a 4 ml aliquat of organic layer Put on Nitrogen Evaporator to dryness Add methanol Volume 1 O Vortex 30 sec. Temperature: Room Temo. TN-A- 3 V t ' Filter using a 3cc B-D syringe with a 0.2 um filter into an autosampler vial Cont. Cal. Verifications used same matrix as for std curve. -------------- 1 -- . 1......... \X 10/12/99 Draft Attachment A ETS-8-4.1 Extraction of PFOS from Serum Form Completion . / Verified By Sam pie W eights/ V ola m es P rop D i t t i ) : 10/19/99 A nalyst(f): SEE Sem ple M atrix: R atScnim M cthod/R cviaion: ETS-8-4.1 T a ra ti Aaalytc<s): PFOS, PFOSA Sam ple ID 9R03230M,DyI,Control 9R03231M,Dyl.Control 9R03232M,Dyl.Control 9R03233M,Dyl.Control 9R03234M,Dyl.Control 9R0324SM,Dy 1,3mg/kg 9R03246M,Dy 1,5mg/kg 9R03247M,Dy 1,i mg/kg 9R03248M,Dy 1.5mg/kg 9R03249M,Dy 1,5mg/kg 9R0323 SM,Dy4,Control 9R03236M,Dy4,Control 9R03237M,Dy4,Control 9R0323SM,Dy4,Control 9R03239M,Dy4,Control 9R03250M,Dy4,5rag/kg 9R03251M.Dy4.5mg/kg 9R03252M,Dy4,5mg/kg 9R03254-lM,Dy4,5mg/kg 9R03254-2M,Dy4,5mg/kg Initial Voi. L __1 O <YiC_____ Study N um ber: TOX-145 Box: 99-206 AF inal S olv en t T N N u m b e r: M eO H /T N -A -2945 M atrix B lank/Idcntificr: Rabbit Scrum/99062-39 Rat Serum/99062418 Verified By: Commenti ________ Wl& _________ ____ M J t_______________ . _-- J _____ \ V, ==---- Sum m ary of m ethod: - .... .......... :7 ~ i n r r ^ ^ y r = --------- -- -- Noies: Review Date RUI0199 I| , O * t`U |i f. ^ so~?* T ir t i| | 3 ^ P n If Mlr '* ` Ml il ss|l Mi -ifl t rU>*n* r * | -t.iS | s | 1 *fi ,5 I 5! f g2SS is* Mil1 2 | sg> i i i s Mii 3 * 8 i ! S i S 3 2 s i 5 ; ; 3 ? 1 O| 'l S }M Hn r ? , r a 325!*H 3S tfSji i i l l l l i i . It ysss U*t H >m> ( > m\11 l i l l i i i l l f5j gfli * Mlfl l a l i i i ? H H H lpi fiP'sf f:i 1 I2SBSSS1s|||| M! M|3* Si-*S f a I S S S s S I S Mi MiS i s S S a s Mi3 3 t 6 s ; : s t Mi Ml -II- 1i*" fcuM Mll i l i l 1 wff Mfi i l l i i i i i Mi0000S0i0S0s5s5 n PPOaaooftD. IC ISfg|fgI^|fe jj ri r*e T* PT <l" V V t 11 rr - r - r r r - - , t 8 8 S2 8 SS8S^|^ Jj iiiiiiiiiP-^fe ii si DILUTIONS SUMMARY SHEET Study: T O X -145 D ilution D ate/A nalyst: M C H , 10/21/99 B ox//: 99-206 ,. Solvent/T N N um ber: M eO H , T N -A -2945 E xtraction D ate/A n alyst: SE E , 10/19/99 , M atrix/T im epoint: R at Sera D ays 1&4 s a m p le n u m b e r o r d e s c rp itio n 1 :5 0 9 R 0 3 2 4 5 M ,D a y l,5 m g /k g D 5 0 1: 1: . 1: . 1: . D IL U T IO N S 1: I : . . C om m ents ti/h 9 R 0 3 3 4 6 M , D a y 1, 5 m g /V g D 5 0 . - .. . 9 R 0 3 2 4 7 M . D a y 1. J m g A g D 5 0 . . .. . 9R 0324S M , D a y 1 ,5 m g /kg D 5 0 .. .. . R 0 .1 2 4 9 M , D a y 1. 5 m g /k g D 5 0 ..- . 9 R 0 3 2 5 0 M , D a y 4 , 5 m g/kg D 5 0 . .. 9 R 0 3 2 5 IM , D a y 4 , 5 m g/kg D 5 0 --. . 9 R 0 3 2 5 2 M , D a y 4, 5m g/kg D 5 0 -._. . 9 R 0 3 2 5 4 -IM , D a y 4, 5 m g /k g D 5 0 9 R 0 3 2 5 4 -2 M , D a y 4, 5 m g /kg D 5 0 -------------------------------------------------- .. ./ - - - - - i/ * V e rifie d B y m l Iz ilff H lff i ___________________ "-- -- /fl/a -f u-- - ___-- -- - V_____ ________ Notes: D50-20 uL sample + 980 uL MeOH. (oj'W " ~ ~ ---------- Form Completion Verified Bv: < & * tC / o k j / f f Extraction Worksheet ETS-8-6.0 Studv # / / V-J Matrix Box# f t - J WK/Dav /V /4- DateSpiked/Analyst -Z. / Z -H206lk -1 -LiverBIk - f -6pph-1 -12ppt>-1 -30ppb-1 -60ppb-1 -120ppt>-1 -300ppb-1 -600ppb-1 -900ppb-1 -1200ppb-1 Surrogate ito FC Mu FC Mix FC Mix Approx ppm : aporox.0.5 ppm. approx.5 ppm approx.50 ppm Actual lei ppm laciual ppm actual ppm actual ppm # Fj * J 2 2 L L J lo/xJ+ r-A t*^ '/ lfa - A + v ' / o/jjA 5 0 ul _____ ____________________ L 5.0 ul I I/ / 5.0 ul ' 2 ul 1 / 5.0 ul 5.0 u: 4- ^ _____` 10 ul I / / / / 5.0 ut 2i i y 5.0 ul 5.0 ul 40 ul 1 / ~ /f\ i _____ T ) ...... 5.0 ul 5.0 ul 5.0 ul / / / 1 20"S 1 30 ul 1 _______ z __________ 4 ul Commeats Verified By \ _____ }/ \ \ .- \ i i =b ' I_____________I_____________ >i !I I ________' } J I_____________ -- _ y oO x fa ? i i / "' " j I! : "---^ Blank __f i i k h b i t y f S __ Std# 9 y - S' Liver Extraction Method ETS-8-6.0 I I amount = /. e> ml g/ml Date & Initials Vortex 15 Sec. Pipette Matrix, spike with appropriate surrogate or FC-Mix Volume , 0 ml Pipette 1 ml of 0.5 MTBA. pH 10. pH= fa /o M t? Std. # Pipette 5 ml of 2 S U I S & X J t m M NaH- bullet Sid K YfYn~,B 2S Dispense 6 ml of methyt-t-butyl ether TN-A- y - f t t . Shake 20 min Shaker speed ^ir>T> Centrifuge 20-25 min. Centnluqe speed: . f f e / l Remove a 4 ml aliquat of organic layer Put on Nitrogen Evaporator to dryness \ emperature rtoom L a m Add methanol Volume //t> ml TN-A- A f 9 J Vortex 30 sec. ___________ _______ , ..-U k llS ? , J Filter using a 3cc B-D syringe with a 0 2 um filler no an autosamcier vial Cont. Cal. Verifications used same matrix as ter stc curve ___________ uL L, 10/12/99 Draft Attachment A ETS-3-5 Euraction of PFOS from Liver Form Completion Verified By A - *r xs-f Z s i s 5 3 ?8 8 T gf 2 XS jl j SX X 11 88! i -n 8 .13 sf Ji XX* f s VJ fl *X X 8 oooocc ooootr -f 8 8 oS "*5 IA 8 8 *,si -? J8 ? ss s *2 . 6 ? B8 8 8 g g g g 8 8 8 8 llg g 8 8 S s s S S s i S bM i Ax !~ s g g g g 8 t|si S 8 o g 1 8 8 8 s *s S iiillS i i *8 M * i e y = w>k 8o8bb?888 t *f, S. * 88 8 a !* 8 S g g g g 8 t g l j? a8 ! " 1 2l f 1 *i i jrt l I UN r - t i 8 V *^V o !r S7S5!2S S 5 s s8| & i*i Vfti 5 | = s 5 c s 5 OOS -8*1 S 5* gSsBcsS = < S g | "PS* a! gSSaEsc *fi 0.5000 05000 0.5000 0.5000 0.5000 5.000 5.000 5.000 50.00 0.5000 05000 0.5000 0.5000 0.5000 5.000 5.000 5000 50.00 O.JOOO 0 5000 0 5000 0.5000 05000 5 000 5.000 5.000 50.00 > ,,i mv*u-9PPP! lisiiiiii hs| V Sail not ' 8 V* S * J' S1 isf x el* VIn o nH f f i ? f i f 2S.X M t Sf if i&? ` i n 'ln 1i r1r1e! pg9 s*8S "3 i s ill! * h * V- V sfc M *5-1 M - o f j r P ^ i ? i l i i i i l i i I P^ n 1 VI {* 9 |= s 5 E5 5 a s f | s 0.5000 0.5000 0.5000 0.5000 05000 5.000 5000 5.000 50.00 Mi z Ss 5 z SE Si l l V) a. 3 SgSsSESS: *? f SP S N> U i c s 1 w m *\P9#0P 3 Insilili uum v00006 (n liiiiiiii tfi 'l{ f aa H oooppooao. " ? g in m '|= ppppppppp P esEEsssEes*!* p ? r*i ? I > I--i Extraction Worksneet ETS-8-4.1 Study # 7 V * 7 ^ Matrix Box# WK/Da> N / QateSpiked/Analyst -H20BC-I -SeraBtk - i -5ppb - / 10ppb - / 25ppb-/ -50ppb - / -100ppb. / -250ppb_ / -SOOppb - / -750ppb - / J ' -1000ppb - / ,,_____ ____ ___ *--------^ Surrogate Std FC Mix FC Mix FC Mix Comments Verified By Approx ppm acprox.0.5 ppm approx.5 ppm approx.50 ppm Actual ppm aciual ppm actual ppm actual ppm # 9 fe y ^ Y t-l # 99tfr-Vfr.l /,A xbr~/tu~ 1 / 5.0 ui i n 5 Out J. _____ Bia____ ____ tif.b_____ ____ _____ 5.0 u! 10 ul 5.0 ul I 20 ul ft ' 5.0 ul 5.0 u! I AdIrt - I iI 5ul 10 ul 5.0 ui 20 ul 5.0 ui 5 0 ul , i _____ 5 ul 10 ul 5.0 ul I 5.0 ul I 'I , IS ul _____ 1/ 20 ul . , J ...- i ____ 4 ___ _____L _ __ I _____ _____________ I . / __ c_ ______ :______ i_ i ------ -- ---------r------------------ f Blank I f f * ___ S\* Serum Extraction Method ETS-8rll - i <X. amount = h O ini..... Oate & Initials Vortex 15 Sec. Pipette IMatrix, spike with appropriate surrogate or FC-Mix Volume j , 0 SeA di*~ ml Pipette mlof0.5MTBA.pH10. pHV/ Sid. # Pipette 2 ml of 0.25 M Na,COj/0.25 M NaHCO, Duffer Sid # 9FtT/.-/`/-oX Dispens e 5 ml of methyU-butyl ether TN-A- jl+YC Shake 20 min Shatter speed; J pg Centrifuge 20-25 min. Centrifuge speed: 3 >&0 Remove a 4 ml aliquat of organic layer Put on t>itrogen Evaporator to dryness temperature Koom Iemc. Jr Add mel hanol Vortex 30 sec. Volume.I TN-A- 1 Y r o l l 3 f o 9 -ff> / Filter using a 3cc B-D syringe with a 0 2 im filler `mo an autosamoter vial Coni. Cal. Verifications used same main* as fo` s;c curve , 1/ . ___ --* -- 10/12/99 Draft Attachment A ETS--J i Kx: K tion ofP FO S rrpm Serum Form Completion Verified By -V*- t o j i T /iS Ion f o r Standard C arve* -Fin d P re p O am ai: Analr*Ui|: S am ple M a iri : M e ilM h d lU crw eo : T a rg e t A iia lp ie ia i: g o t Num ber: iivism *WW / ? 4, RM hi Scntm ETS-t-l I Below 9-206 . .. / Slndy Nambnr. TOXI45 t t | n iy o n il Nom ber: Final Salem l A TN .Somber? MeOI/TN-A-l4S Blank Tiaaoo/ldeattfkr: R iM U Scra/TOA-2J*2 FC Mi Std Approa. 0.500 ppm: F C Mi Std Appro*. J 00 ppm: FC Mi St4 A ppras. 50 0 ppm: S n rrtg * 1* S d Approa. 101 ppm: 9 9 0 16 -U -J 9906-44-2 *906-44-1 9 9 0 6 -l3 -ll AemaJ Conccntranooi o f Standard* m (Be FC M i * __________________________ _ PfOSA EtFOSEOH MSS* MS7* Std Cone Sid Cone S*d Cane. Sid Cane uif/mL 05000 ug/mL 0.3000 ug/aL 0.3000 Hff/mL 0.5000 0 5000 0 3000 0.5000 0.5000 0.3000 0.5000 0.3000 0.5000 3000 5.000 5.000 5 000 3.000 5000 5 000 5.000 5000 5.000 50.00 5.000 50.00 5.000 50.00 3.000 30 00 50 00 50.00 30.00 50 00 50.00 50.00 50.00 50.00 50.00 50.00 50.00 soar 50.00 M rfO SC O H lid Cone. ng/aL 03000 05000 0.3000 3.000 3.000 1000 30.00 30.00 50.00 50.00 gUnk aentm initial roJoa* (a L I Ur enreaa: Fim l w lw m n l i w (mLl far enreea: 1.00 1.00 POAA S d Cane 05000 05000 05000 3.000 3000 3000 50.00 50.00 30.00 50.00 PFHS Sid Com:. ng/mL 0.5000 0.3000 5.000 5.000 5 000 50.00 50.00 50.00 50.00 Am f Spiked mt 0.010 0.020 0 003 0.010 0.020 0.005 0010 o o ts 0.020 All Initial Volume ml VALUE! I.OIS t.025 1.010 1.015 1.023 1.010 1.015 1.020 1.023 AH Final Vpl. ml 1 000 1 000 1.000 1.000 1.000 1.000 1.000 1.000 1.000 1.000 Calculated Coaccatm p ro s Std Cooc PFOSA Std Cooc np/mt VALUE! 4.93 976 97.6 97.6 24* 241 493 735 733 976 976 EtFOSEOH Sid Cone VALUE! 4.93 9.76 24 1 493 97.6 241 493 735 976 MSS6 Std Cane. ag/aL VALUE! 4.93 9.76 24.1 49 3 7.6 24 493 735 976 MS70 Std Caw. gfoL VALUE! 4.93 9.76 241 49.3 976 241 493 733 976 MeFOSEOH Std Cone. ftaL | VALUE! 4 93 976 24 49.3 976 24 493 715 976 POAA Sid Cone. VALUE! 4.93 9.76 24. 493 976 24 493 735 976 PFHS Sid Cone. a/mL valUe ! 4.93 9.76 24. 49.3 976 24 493 735 976 arrogate Std Co m . ng/mL All Am t Spiked mL S em filr Final Cone ag/aL 49 PFOS final Cooc. ag/m l VALUE! 300 too 23.0 100 230 300 750 1000 PFOSA Final C o w ag/aL VALUE! 5.00 100 23 0 500 100 250 500 750 1000 EifOSEOU Final Cone. ag/aL VALUE! 5.00 10.0 25.0 50.0 100 250 500 730 1000 M3S6 Final Oroc. ag/aL VALUE! 5.00 10.0 25.0 30.0 100 250 500 730 1000 M510 Fmal Cane. ag/L VALUE! 500 10.0 250 500 loo 250 500 730 1000 MeFOSEOH Sid Cope. ______________ IVALUfe1 5.00 10.0 25.0 50.0 100 250 500 730 1000 POAA SdCoac. VALUE! 500 140 230 500 100 230 500 750 1000 rru s Surrogate Std Cone. Std Cone. , . H '* l ____ VALUE! taL 101 3.00 Surrogate 10.0 Fmal Cane. 23.0 ng/aL 30.0 303 100 230 500 730 1000 All Am't Spiked aL 0005 Sample macd for MS/MSO: NoMS/MSD MS/MSO Cone, in the tample mamu PFOS PFOSA Final Cone. Fmal Cone. ng/mL ag/aL 24 24 24 24 EtFOSEOH Final Cone. ag/aL 24 24 latdal V olnaetaL ): 1.00 MSS6 MS70 MeFOSEOH F a il C ate. Final Cone. Std Cone. ag/aL ag/aL ngML 24 24 24t 24 24* 1 24 2.00 POAA Std Cone. Si:__ 24 24 Appro*. S d Cone.: 50 ag/ml PFKS Sid Cone. m/mL 24 24 Sample warn* for MS/MSO: No MS/MSO MS/MSO Cane, la tfce fmal tolveat_______________________________ Initial Volume (wL): 00 PFOS PFOSA EtFOSEOH M3S6 M37 MeFOSEOH Std Cone. Sid Cane S d Cone S d Cone. S d Cone S d Cone. ugfrnL ng/mL ng/aL groiL ng/aL ugrmL 250 230 230 250 230 230 2JO 230 230 230 230 250 2M POAA S d Cone. ng/aL 250 230 Appro* S d Cone SOup/ml PFHS S d Cone. ng/aL 250 230 Ain't Spiked Voi. (m t) 0 003 A m t Spiked Vl (*L> 0003 Final Vl. ( n i l I 00 IPSE*l02J9Sei-9906-U.| xH JO /jf/tf Prep Oiliest): / M i l .M t a ly illu : S am p le V lucrti: "Jtirtt'Y. ft* M cttioil/R cvision: T a r s e t Analyte**!: ffZ& J f b A ^ Sample Extraction Sheet Study N um ber: Equipm ent N um ber: N otebook* anti Puce: Final Solvent: #J-A - 7 7 ? Procedure O euil .TTirxtM. __k!- ....J iJ h __iH * . pA '* < Jim **. t- f t __ (n * J - / | 'A t___ L u a & L ***nJ-. Tin, b lin k !I *T C rr f>U* utuL. ?O A*/7Ft> s - 7 f m - 3 7 - - ^ s * J - T sn> -- fto lt -13--!I JqJ * fr J b m XTA> V& S g f /T - Vf ' 'fc t/P o A A (+ r d (B F * .v- J W it es_ *->*<*> * --Z *^ L 5 iiZ 5 Z Z ic . y * x Aoo x, __jg P b f p L Z& 4 ^ - X /B o ? -X A . / o o Extraction-! Template Review D ate_________ EmporefcxtracuunP3.xls Page I ot S am p le E xtraction Sh eet P rep O liteci A nalyxtfx): tAS a m p le M a tr ix : ^ T < f . M ethod/R evision: Target Amilytels):^#*/^/^* ___ _________ ?f**A------- Study Number: 7o Equipm ent Num ber: Notebook# and Pace: Final Solvent: - JftA - f t { P ro ced u re D etail *7L- 7 iV - A - tf - S - U S ~ -> L > --+ 3ofl> i "-i. ^. ^ / _f /f,m_ j/. / . m .1/ . /* //// ala.. d + 'Vi .jj* 6 rt g ^ J ?oAA l,*.+a - f i * .. '5 `f lx s __ tir $ / f - L l. ojha v -hJ ' . / 7^> ...,^y i M J W > 7 ___* * -d Z V ` 7fcac-w . JtSeuE & s^ o**Lfi<e f _ a a/* A m : / e U Y . . -- a!d____ 71. !!** 1 t / * r k - S u K rt.j4*c- SU> M~tJ _________ __ ________________________________________ e r r o r i - / * - c * j u . ! j r v _~~'*y> ^ __ T fa j/h iA A - m u - 3* 3 -* * . */ 7 P ~ /T t AA ..................................... ] T^r*. /pod < /a a w . '*'^~^** c~ y -4 -- T W <__ /tftfg * * a> -x.__ - u A bx>~L. { - + t e a s * o . 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V {< (hotl/R *iiM ii: T a rg et 7b*+/yf*> P ro cad u ra D atati Sam ple Extraction Sheet S tudy N*mb*r- /> > . t* /S .NtamlMr: anil Page f `"* l ^ J/V r v - a - Vj rfyfA So-m L J - ( f*~--/ V * 1 ' 7 ^ r ^ <f ...c^--f ` '< v n4.OL /*- ..ard*-*r -A - 'H/><j*7" ^^ ~!'-*'** 9 "j VXa t= -u tr * -----hKaSlf-----S-*U --d--*--<--r------A------ U = i i ----;1M ,------y . i H iti* . -ilu td - t L * / Iy*c-*r-f7 Ac---- -d L -- I t * , / ' t ___ ~R*- /> l(-` i*l'Vj atfn dt*< `~* V - .CXt__ <L S& * x ^ J T fgS. - f3X& - n - t # f r f /PO /**. - <Ut> * o 7* q S ' / x > a * ~ f t * A - s r ~3 * t f f l i j ~~ d j* >^6w> ^ /^C* FFo s /F oaa- - .Hf- ' ,/ga6-- * ^ g - H g J r O // / t-i. 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J C P 9 * .''< J '/ * S r s / Al. / O H ^L -r J <* <?, u - r ___f _______ x d S Z s r ^ A ,_____________________ J ________ traction* I T em plate M<v* Oate Etraction Il Form .Approved byTTauT Pige l ot' _____ Extraction Worksheet ETS-8-4.1 Sturtv # TOX 14 5 Matrix Rat Sera IJox f 99-208 WK/Dav Dav 29 DateS piked/Analyst RBSl 1039-250ppb-CCV9410 R T S 1 1 039-SOT0ft*9&10 RTSl1039-250ppfr-MS9 RTS11039-250ppt>*MSDlO RBStt039-H2Ok-9*t0 RBSll039-Sr#Blk-9410 Surrogate Std FC Mix FC Mix FC Mix Comments Approx. tOOppm approx.0.5 ppm approx.5 ppm approx.50 ppm Actual ici ppm actual e.-; ppm actual. c ppm actual ppm 'ttO cIv-iV il 4 J/JA U lO JlM 5uL m - a # ` M.; >?i(.--f-J-l -- .------------- - - 5 uL U l . u ;i l o i l i 5 uL - - ' 5 uL - - 5 uL 5 uL - - 5 uL 5uL - - - 5uL -- Verified By I______ RBSn039-5ppb-9A10 RBSU039-10ppb-9&10 RBS! 1039-25ppb-9410 RBSl1039-50ppb-9S1D RBSl1039-lOQppb-Mt10 R6SH039-250PPC-9410 RBSl 1039-500pp0-94l0 RBSl 1039-750ppt>-9410 R8S11039-10Q0ppb-9410 9R03240M-0-Oy 29 9R03241M-0-Day 29 9R03242M-O-Dy 29 9R03243M-0-Oay 29 9R03244M-0-Oay 29 9R03255M-5mg/kg-Day 29 9R03256M-5mg/kg-Day 29 9R03257M-5mg/kg-Dy 29 9R0325aM-5mgA<g-Day 29 9R03259M-5mg/kg-Day 29 3lank: Rabbit Sera 5 uL 5 uL 5 uL 5 uL 5uL 5 uL 5 uL 10 uL 20 uL ' - 5uL 5 uL 5 uL 5uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL 5 uL | HZ | - * - std# p | C t o v a 'cfn -- 5 UL 10 uL - 20 uL * - 5 uL 10 uL - 1 5 uL - 20 uL -- -* -- --- . _ - -,- -- amount = l.O ml ... \ \ ______ s L y ta Serum Extraction Method. ET S-4-4J. Oate & Initials Vortex 1 5 Sec. Pipette Matrix, spike with apprc>pnate surrogate or FC-Mix Volume i . 0 ml Pipette 1 ml of 0.5 M TBA, pH 10. oH= i n i f / t / i e S t d . r H 0 M , - ) H t S ____________ %t ______ Pipette 2 ml of 0 .2 5 M N a,C O y0.25 M NaHCO, buffer std . < w m u iia - o * . Dispense 5 ml of methyFt-butyl ether TN-A- /WMlij Shake 20 min Shaker speed: 3 *t " Centrifuge 2 0 -2 5 min. Centrifuge speed: 35QLrem Remove a 4 ml aliquat of organic layer Put on Nitrogen Evaporator to dryness 1 emperature: Room Temp. Add methanol Volume '-u ml TN-A- r f - - Vortex 30 sec. Filter using a 3 c c B-D syringe with a 0.2 um fitter into an autosampler vial Cont. Cal. Verifications used same matrix as for std curve. ///m e -- KJ/ A, VY---------- -- ^_____ FN-1: The MS/MSD and associated sera blanks were taken from control rat sera TCRclc(Cv'i 'h C 10/12/99 Draft Attachment A ETS-8-4.1 Extraction of PFOS from Serum Form Completion Verified Bv //AVR id - * i Ion Pair Standard Curves-Serum P rep Datcta): 1 1/03* A u lv il(s|: MCH Sample M atrix: Ral Sera Metfeed/Rcviaien: ETS-l-4.1 T arg et Analyte!!: PFOS. PFOSA Be N u m ber. 99-201 Study Number: TOXHS Equipm ent Number: Futal Solvent * TN Num ber: MeOH TN-A-2997 Blank Tiaaue/MeuUAcr Rabbit Sera TCR99062-94 FC Mi Sid Appro*. 0.J0Q ppm: 990*6-47-2 F C M il S td A p pro*. 5.00 ppm: 990*6-47-1 F C Mi Std Appro. 50 0 ppm: 99095-53 S u n r |t(e Sed A pprox. 100 ppm: 990*6-13-11 ram initial vekame (m L) fa r curvea: Final solvent volume fm L) fo r curves: 1.00 1.00 Actual Concentration* o f Standards in the FC Mix PFOSA PFOSAA EtFOSE PFOSEA MSS* Ail All Std Cone. Std Cerne. Std Cane. Std Cone. Std Cone. Am t Spiked Initial Volurn Final Vt. 4 0.5000 0.5000 3.000 ug/mL 0.5005 0.5005 5.005 5.005 ug/mL 0.4997 0.4997 4.997 4.997 (/m L 0.4999 0.4999 4.999 4.999 ug/raL 0.5005 0.5005 5.00$ S.O0S uii/raL 0 J 0 10 0.5010 $.010 S.010 mL 0.010 0.020 0.005 0.010 mL 1.025 1.010 t.o is mL 1.000 1.000 1.000 1.000 5.000 5.005 4.997 4.999 5.005 5.010 0.020 1.02) 1.000 50.00 50.00 30.00 50.00 50.05 50.05 $0.05 50.05 49.97 49.97 49.97 49.97 49.99 49.99 49.99 49 99 $0.05 50.05 $0.05 50.0$ . $0.10 50.10 $0.10 50.10 0.005 0.010 0.015 0.020 1.010 1.015 1.020 1.025 1.000 MOO 1.000 1.000 Calculated Cooccniraooiu o f Standards in the sample mam* PFOS PFOSA PFOSAA Std Caoc. Std Cone. ng'm L o c ta l. 4.93 4.93 4.92 9 76 24 8 9.77 9.75 24 1 24.7 49 J 49.2 97.7 97.5 24* 241 247 493 493 492 735 736 735 976 977 975 E tFO SE Std Cone. ac/m L 4.93 9.75 24.7 49.3 97.5 247 493 735 975 PFOSEA Std Cane. ngtaL 4.93 9.77 24.1 49J n r~ 241 493 736 977 MS5* Std C o ac agtaL 4.94 9.71 24.1 49.4 97.1 24* 494 737 971 S utregate Std Cone. ug/mL 101 S u rro g a te Final C o n e ogtaL 491 AH A m t Spiked mL 0.005 _ rt C a k u lu e d C o a c m m iiw u o f S u o d u d j ia dK 1.0 m L Goal lo lv a u v a ia n c PFOS PFOSA PFOSAA EtFOSE PFOSEA M556 S u rro g a te AH Final Coac. Final Cone. Final Cooc. Final Coac. Final Caac. Std Coac. Std Cone. A m t Spiked ng/mL ogtaL ng/mL m/mL ugtaL ngtaL ug/mL mL 500 5.01 5,00 5.00 5.01 5.01 101 0.005 10.0 10.0 10.0 10.0 10.0 10.0 S u rro g a te 25.0 25.0 25.0 25.0 23.0 25.1 Final Cooc. 50.0 50.1 50.0 50.0 SOI 50.1 ag/mL 100 100 100 100 100 100 505 250 250 250 250 250 25! 500 501 500 SOO 501 501 750 7SI 7J0 750 751 752 1000 1001 999 1000 1001 1002 Sample used for M S/M SD: TC R99062-50 MS/MSD Cone, in the sample m a w PFOS PFOSA Final Cone. ng/mL 2a 241 Final Cone. ng/mL 241 241 __________ PFOSAA Final Cone. `p * L 247 247 Initial Volume (m U : 1.00________ EtFOSE PFOSEA MSS* Final Cone. Final Cooc. Std Cone. ng/mL 247 ng/mL 241 __ a s i __ 241 247 241 241 Appro*. Std Cone.: 50.0 ug/mL A m i Spiked Vol. (mL) Sample used for MS/MSD: TCR99062-30 MS/MSD Cone, in the finad solvent________________________b ntui Volume (mL): 1.00 PFOS PFOSA PFOSAA EtFOSE PFOSEA Std Cone. Std Cone. Std Cone Std Cone. Std Cone. ug/mL ugmL e 1 r ug/mL ug/mL 250 250 250 250 250 250 250 250 250 250 M5S6 Std Cane. ug/mL 251 251 Appro*. Std Cone.: 50.0 ugm iL A m t Spiked Vol. (mL) 0.005 Final V oi.(m L) 1.00 T axIt5 itih ''-'1 DILUTIONS SUMMARY SHEET Study: T O X 145 D ilution D ate/A nalyst: 11/5/99 MCH B ox #: 99-208 sam ple num ber or descrpitlon 9R03255-5mgAg-Day 29 9R03256-5mg/kg-Day 29 9R03257-5mg/kg-Day 29 9R03258-5mgAg-Day 29 9R03259-5mg/kg-Day 29 1:10 DIO D10 DIO DIO DIO 1: . - . . ,c ``P I 1: nn . . . 1: Nfc . _ _ / ___________ / ________________ L___________________ V Notes: 010=100 uL sample + 900 uL MeOH. ^ Il|<i So l v e nt / TN N u m b er: M eO H T N - A - 3~V gk Extraction D ate/A nalyst: M C I! 11/3/99 M atrix/T im epoint: R at S era Day 29 1: ha - DILUTIONS IfJe. 1: yJtv . -. . .. 1 . __ . . Comments Verified By N /ft 1_____________ \\ \ \ \ \1 j \ \ 1 1 s L _ _________ \ \ 1 4/ Form Compjgtion . I j Verified By P J k A 11 \ 1 Extraction W orksheet ETS-8-6.0 Study i* TOX-145 Surrogate Std FC Mix FC Mix FC Mix Comments Verified By Matrix Rat Liver__________ Approx, ppm approx.0.5 ppm approx.5 ppm approx.50 ppm Box# 99-211 Actual/// ppm actual ppm actual ppm actual ppm WK/Oay Dav 29 # W a l l /-V/ # 7 9 & c - w J # # S // OateSpiked/Analyst h/j A * - / w &//<?</9 ~ -CCV-/-/,,/-2_ 5.0 Ul -m s - 5.0 ul / -MSD- 5.0 ul (U, // ,, V -H20BIK-142 5.0 ul (is s (f/jki / 10 ul 10 ul 10 ul / . ({/A ffa ).. ... ______ / ____ _____ J ________ / ____/ ! _ V / _________ Ulu- nfonf1! -LiverBlk-1&2 5.0 ul / // .Lift______ -6ppb-1&2 -12ppb-1&2 5.0 ul 5.0 ul 2 ul 4 ul / / / / _ -30ppb-1&2 -60ppb-1&2 5.0 ul 5.0 ul 10 ul / - / 20 ul / /n -120ppb-1&2 5.0 ul 40 ul / ________ -300ppb-1&2 5.0 ul / 10 ul / -600ppb-1&2 5.0 ul A O 20 ul / -900ppb-1&2 ^ -1200ppb-1&2 5.0 ul 5.0 ul A / A 30 ul .Z___________ 4 ul / / t/ Sample numbers and weights noted on a separate page - add 0 ul surrogate to all samples. -------- - 7 - - ft* 1*17*7 *V* ^ ---- ' , - r -------- . Blank -/? j j , f *C_, SU* amount * A > ml Vortex 15 Sec. Pipette Matrix, spike wrth appropriate surrogale or FC-Mix Volume. Pipette 1 mi of 0.5 MTBA. pTTol std. m* g/ml - m.u- il)H |^ Vortex 30 se c Filter using a 3cc B-D synnge with a 0.2 urn filter into an autosampler vial Cont. Cat. Verifications used same matrix as lor std curve. 10/12/99 Draft Attachment A ETS-8-6.0 Extraction of PFOS from Liver Form Completion Verified ByJ j j j d j j f s d k * ) P rep D an is): 11/3/99 A na ly stia ): RVVW Sam ple M atrli: R at Laver M ettaod/Rcvisio: E TS4*i.O T arici A ailyted): PFOS. PFOSA Sam ple ID 9R03240/M /Day29/Control 9R0324 l/M /D ay29/Corrol 9R03242/M /D*y29/Conirol 9R03243/M /Dy29/Comrol 9R03244/M /Day29/Conin>l 9R03255/M /D*y29/5ra*/kg 9R03256/M /Dy29/5m */kg 9R03257/M /Day29/Snig/fcg 9R0325i/M /D y29/3m g/kg 9R03259/M /Dy29/5m g/kg Sample Weights/ Volumes laitial WL E ///?> . hJH /.flifO / , I J r ...... /f C-f M Q W ater ml 5 ml 5 ml 5 ml 5 ml S ml 5 ml S ml Sol 5 ml S ml Study N um ber T O X U 5 Equip* Num ber; Fiaal Solveai TN N um ber: M Q W*er M atrix B laak/Ideotlficr: R abbit U vir/W O I6-IJ-5 Boi: 99-211 Verified By: Com m ents -- ---------------------- -- --------- ? x J jh _____________ X u n 1 '_________ X _________ --------------------------- ............. -- } ____ C ------------------------------- _ _ _ ------------------Sum m ary o f m ethod: Notes: R eview D ate Form Approved by/Date: W eight Volume Sheet-IOI299.xls Form Completion Verified By: i l l 1.00 1.00 200 '5.00 3.00 10 0 10.0 20.0 20.0 30.0 30.0 100 100 130 130 200 200 300 30.0 81 *r2 r E 32t a *?* l iu t 1.0 L f i l l alvo* w l t M8 8 e e H [I * ag 8 8 , oe sf! s s a* e e "io S! 2 s f! 32 ifi siiSisfca l iSSSSi fis 2.00 Ssiigggg[ fm 8 O 8 Q i. 1r*s 23 il* ? l i | l8 8 O '6 X 8 33tp i m B x iggi S S i g! U\ M t.oo 2.00 3.00 10.0 20.0 30.0 ICO 130 200 88 e *?? 22 m > 88 OO 1 32 issgggsssi M 1 t- |l *i G pl s; I 9 I - sbc E no - *i 0)000 0.5000 0.5000 0.5000 0.5000 5.000 5.000 5000 50.00 uugiw e e e o e 1 ss i i i IrI 11 ! .t lii " rsss 4h * U . ititu r! | n i S |? ? *i fit !* '5 s f s p S* SIp- IA- " m JB a - m l i 5 f -> * 1 t *Wt*U,5PPP , . i : i s i i l l i l i Iffg S S S s E s c = I sf l 1 i i i i i i i i Sfi5 S tiS H d =iPf |n ! uuw uioee 1 i 1111Sfig S S S B S E S S SS 1 W UW lPPPPP gssssn g es, f e |i g i= B E ! 3SssSSf ilg 11111i i Ms Z Ili'lli i iff !| iisiillii l}i il !! it M V> .| 3 H ie o o e e o o o o S M> --o ii i 8ff OOOOOOOO aaa I? f UMf3i t r* X "1 S i I 1 DILUTIONS SUMMARY SHEET Study: TO X-145 D ilution D ate/A n alyst: SA L 11/9/99 B ox #: 9 9 - 2 1 1 Solvent/T N N um ber: MeOH TN-AExtraction D ate/A nalyst: R W W It/4 /9 9 M a trix /T im ep o in t: Rat Liver D ay 29, Grp 6 FACT: DATA REVIEW SUMMARY FORM Date: D ata Analyst: D ata Review Sign-Off A nalyat Review N a m e /D a le : _ 3 _ i 2 2 l i a s ___________ FACT Study*: M atrix/Tim epointa: S Sire. --Thy ! j 4 - i<<1*** Il/rs ?& T echnical Review N am e/D ele: tf)E M S~"ptUt Set-up Analysts Date/A nalyst Instrum ent to n fila ____ ,. ----------------------------------- t9/t1n1 MkM ^au^p 07- __ _ A iiaS te : 7oAA (CHtlP A cceptab le L in e a r R a n : AM I.O O : A lA S * i C+*UKtif E x tra c tio n B lan k : A/A Q uality Aaattrm ncc R eview N am e/D ale____________ Data Entry:. A A L c ___ l o h l l f t Comments / Joatificarioni: 0 A Cwt tats a ../' ru * t / d L -/it. a d u s i* J - 7*A.---- A f (L /f. J f } j f e e h a k n j a/ tr e e . i t d c -- R A2: A/A Calibration Cheeka: A/A M S/M SD: &lf~ iv t D ata Status: eft* M a trix B lan k : AtA S i L rx n aiiM .n l'f Mo lo jvlfy 71+ -1S mL p a d UtS dr,M>e/________ brcaKSt i-f u tr CaJsiJc. J L h*** tv* ft__ 0+1 -JL Curile <r pA w ___ litrey over T frw s / s ____ A n aly te: TfoS ((Hz') 7t >*LA cceptable L in ear R ange: ^ LOQ: I X f f L Extracted Blank: / w s 4L**. 03 R"2: 0 m - / 0 M atrix B lank: in a J L t* . 06} C alibration C h o c k * f niK ~/j% * / * / y M S/M SD D auStatua: J lL . D . k W r h r iA li r f i o t t i Q nim ftli v.wh WA n a ly te : fcoSfl f W - r ) A cceptable L in ear R ange: t ' $3, t+b L O Q :. 0R A2 : tK ffL ___________ f)KC alibration C h eck s: - M S/M S D : SL Data S ants Extracted Blank: in s 4b> * 09 M atrix Blank: less 4ht- LoQ Ar->** --/3% * / "/* UC -? ibli'I'Jj it 4L HtiO i/tje s f,//,v/Xj -Ah e/o sd _______ Sar^Us. A^eej *4 4L A d ___ k .jit area S a u d i d * J uiCre OtMttfe------- & ^ ~7L ?3^lr duel p o i d s _________ j/Trt JvotPfJ m *^4L Cart* creuse-_______ 4Lu__tirre auJsiJc 4L l/rs.r- renjc, 7kt Mitt! JeeJss Ix^J ki^L l e d af?FSA. ' X,* " / z .j f f _______________ ?t>A A . A t d M / ^ A gA & /LflM cat\-._____ Q u iu M h A ttM l u n L tiL t d ^ r j u l CUAifCa S ^ ^ frJ^ v e id ( r r * (d rvt/y tita e i f t r ftid o , A E w t a y y ^ Ur J lL d tA . (L iu tu t-- Y f M A '_______ f r * I l 2 l 3 ________ FACT: DATA REVIEW SUMMARY FORM Date: DataAnalyst: X tS FACT Study#: M alhx/Tim cpotnU : ,S / i- 4 .-jiy I f / Samplelist Set-up Analysis D aic/A iulyit: Initnuncnt: H n /ff MAM a2ilK f -<*/ % h l ^ A aalv te: j s CcH*f HAcceptable L in e ar R an g e. a LOO: R"2: MA HA Calibnlion Check#: M S/M S D : Extraction Blank: / /A M atrix Blank: HA ___ / A Data Status: s *-- ^ Data Review Sign-OfT ' Aaalyit Review Nunc / De: 1 * * /y W f t_______ Technical Review Name/Dele____ Six, jia^L t ftF3- QualityA n n u e t Review Name/Date:__________ iAC lolnh"} D ata Entry: l A t l o k l i W Comments / JustUkattoBs: ^ J.tJjftLM.i I**jc L slL . A lL & ^ jtL s . C*n*s 4 c J d t t k i U </eut*J * .i o t &>% o r / V i -- ay ' % / f f ________________________ O u M til/ On^aaart a mIir y MMR T O U I J - m M r . day 1 4 . M t r a l 10/19/9* nrinrl I H a t : C: V K M *tnO C \aM p-ata.|W \aM B 9lnO B \il**b u m M im d i m d o a i t u t i i i m *e*ed: C iV R XBBfcE NX 5aapr-irata.R raM *R ttaB*V l0lt*b U K a a x liC la d i W O JO M U M l* * * Ml OMU: rri 4 : m a c t a m .-oojjo * it rou to il * IM i 1 101*9*012 2 101999013 3 101999014 4 101999019 9 101999014 4 10199901* T 101999010 0 101999019 9 101999020 10 101999021 11 101999032 12 101999021 1) 10199902 14 101999039 IS 101999034 14 101999029 17 101*99030 1 101999039 19 101999030 30 101999011 31 101999033 21 101999032 33 101999034 24 10199903S 2S 101999034 34 1019990)7 27 101999014 30 1019990)9 39 101999040 30 101999041 31 101999042 32 101999043 33 101999044 34 101499045 IS 101*9904 34 1019*9047 37 101999040 30 101999049 39 1019990S0 0 101**4031 41 101999052 1 1011*4053 4) 10119405 44 101114055 45 101944054 46 101994057 7 101994054 44 10199905 49 101999040 30 101499041 51 101999043 52 101999043 S3 1019*9044 54 10199*045 55 103999044 5* 101999067 57 101499040 51 101999049 59 101999070 40 101949071 41 101t99Q73 *J 101999073 dMMlallac Tk mem Blank mem Blank m m Clank TOH4S-RBS10194-E2Q Blank-U. SET TOZlS-RSS20l9*-*ara B lank-ll. S ll WH-*TS10' -i rt Blank-U. SEE TOX14S-RTS19191-Sara Xlank-12. SEC TOSaS-dB*10l*9-5ppb-li. SEE 9OX14S>MS10;99-2*t>-ll. IKS TQX14S'RBSl0l99-2Sppb-11. SM TOX14S-kBS10l99-50ppb-ll. SEE TCZ243>UE101|*-100ppto-ll. MB m U S 'M S lll9 f< 2 S p p b -U , SEC TCX14S-k*S19l9-S0appb-ll, MS m i 4 m . M IJIUK. PyZ, Coacrol. -10/29/99 SEE n Q t i 'I T S , 9M3213M.. Oyl. C M t n l . -10/19/99 ESS TOKMS-RTS. 9E0J234M. Oyl. C aacral.-10/19/9# CSS TQXl4S-*M10144-250ppb-CCV-ll-l. SEE HaON Blank taniS-ETS. >a71233N. Oyl. C o o tro l.-10/19/4 SIS TOXllS-kTS. I M m iN . 0y4. C an tral.-10/19/94 SEE TOE14S-trs. tR0323?K. o r * . C o n t r o l . - l o / l t / f f BBE TOX145-RTS. 9X0123!. Oy. Coacrol.-10/19/99 BEB TQU4S-ETS. 431231. Oy4. Control.-10/14/99 BEB TOX14S-EBS101M'23Cppi-CCV-ll-2. BEB NaOO Blank tOU4S-RTS1319-2Sappb-HS-ll. 10/19/99 SEE TOH4S-ETS13199-2SOepb-HSO-U. 10/19/99 BBS TOX24S-RTS. 9X02245. Oyl. 5 np/fcp 10/19/9* BBS TC0CUS-RTS. 9X03244. Oyl. 5 ap/kp 10/19/9* BBS TOX14S-RTS. 9X03347. Oyl. S M/k* 10/19/99 im TOX14S-RBS10l9t-23Qppb-CCV-ll-3. ( t l H*ON Blank TO*:45-RTS. 9X32214. Oyl. $ op/kp 10/19/99 MB TOK14S-RTS. 9X03219. Oyl. 5 ap/k 10/19/9* BEE TCZ243-RTS. 9X03230. O y * . 5 Op/* 10/19/99 BEB TOXI45-RTS. 9X22251. Oy*. 5 ap/kp 10/19/9* BBS TOX145-RTS. 9X03252. Oy*. 5 ap/kp 10/19/99 BBE TOX:*5-X0Sl3:91-25Cppb-CCV-ll-4. BEX aCK Blank t c x u s - rts. oy, s ap/kp i o / n / i SEE TCX145-RTS. By*. 5 ap/kp 10/19/94 SM Tox;*5-xxs:c>;?>-2s;;pb-ccv-n-i, see HtCM Blank TCZ145-R8S10149-R2O Blank-11. SEE TOXlS-XBS17l)9-Srr* Blank-11. SM TCXliS-RTSUlD-Snrn Slank-U. SBE TOZl4S-XTS10'.9-Sra BlaAk-13. BBE TOXl-XBSia:9-5;pb-i:. BEB n U ( S - M S m M C ;; a - U . BEE TOE115-R*Sll7l-2SppO-ll. SEC TOX14S-RBS101*9-S0ppb-ll. SEE TCXt4S-RXSm9-130ppb-ll. SCI TOZ:4$-RBS10:99-3SQppb-ll, SBE TCX'.JS-KBBlOm-SOCppb-U. SEE TCX145-RlS1019-73Qppb-U, BEE TOX1*S-RB5H191-10Q0ppb-ll. SSI Ty*a tu n ta rt I t aortard Standard Itu lirt Braartard Braartard Braartard St aw ard Standard QC QC oc oc oc Braartard Icaadtrd Btaartard Braartard Braartard Staadard Btaartard Braartard iraorta rrt H 4 Onoo K 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 7.005 7.133 9.133 7.113 7.BB4 9.111 7.109 9.100 9.113 9.110 9 .I ll 9.113 7.111 1.00 7.090 9.111 7.110 9.006 7.111 T.0I9 1.00 7.113 7.113 7.139 9.113 9.104 9.105 1.00 9.133 7.133 7.090 9.111 9.U 1 7.107 1.00 7.104 9.0*0 7.300 7.103 7.110 7.111 1.00 7.110 7. U3 7.U 1 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1-00 1.00 7.109 7.139 7.110 7.0*1 7.113 7.13 7.133 7.111 7.12 9.121 7 .Ill 7.107 7.110 7 braa riapa cuatc. taDarv )7 m 30 NK 34 mm 31 RN 35 tab 42 bb 33 bb 42 bb 39 bb 39 bb SI HH 42 bb 60 Ml 10 MR 37 bb 56 ht> 43 m 43 MR 34 01 39 tab 37 RK 34 MX 33 bb 30 RK 40 MM 5 M< 35 bb 301 bb 25 bb 340 bb 42 bb 391 bb 340 bb 310 bb 20* bb 340 bb U bb 240 bb 334 bb 39 bb 30 NK 30 bb 2 bb 44 RH 31 RM 37 MM 34 Ml 60 RN 37 1M 45 NK 37 RK S3 bb 64 bb 0.00 0.91 0.11 0.90 0.13 0.94 0.7-7 1.00 0.93 0.93 1.31 1.00 1.41 -12 -9 -14 -10 -17 -l -33 0 -0 -7 21 0 41 0.71 0.07 O.B5 1.00 1.03 O.B1 -29 -13 -19 -0 3 -14 0.6 0.06 0.01 0.T7 O.T) 0.94 -32 -13 11 -2) -21 -4 1.32 0.03 7.20 30.04 t . 52 3.00 33 -17 34 *06 752 -0 4.14 0.04 4.97 4.93 4.15 0.73 SM 704 397 193 515 -37 5.61 5.55 0.92 404 55 1 0.44 0.49 0.44 2.04 0.93 0.07 0.01 0.15 0.00 2.09 0.19 1.2 1.51 -34 -11 -34 4 -27 1) -15 -5 -11 7 -13 36 51 1 ow p 0 2 0 t * f r O m i l f l K a d p r l u x l t r l 1 0 /1 9 /0 9 } SS-'T '" S t SSf-fS?' sssssssssassssssssssssssssssssaaassisssssggsssssssssspssss iiiiiiiiTtiSiiUSiaiiSiSiSiStiStiSSiSiii3iiiSSSli ia ^ s s s 3 s s iir s9 rS 3 3S3ss:s,ti ::3 i i ! i I i i i i i i i s S85 s s s s 5 i i | | | i ::::::::: s J - in i i gSSSSSSS l 'SSS255 8 H S BS2EB SEBEE SES ESSES ? ! iSSS l?U 1! a SS5S a.SSSd.sasSSSS8 SssllsS|sfe 5231.....u \m ii= m a n ti a u N k 3 --------- 7 ss' ssp?* nHjrS . ESSE S 1s.s"'ri. hv.~llili UP? 3Sv 252:4:i vvijsv iiyyv ::::.; '??vvvvvvvv s Ur. F.HEssaswr; y?. 5r.?.s:;?.5Ss3s5 ssssssssssSsssssssssssssSs"; S3333335S5SSKSSK5KS5SS33SSSSS5S3535SSSS5SSSSSS5S;S Oannclfy ItM H ir Import 1 0 U tl n *> 4*y 1 ft 4f M f.ira; t Pa- M p l a U lti C:\M*mm>iC u:>.niVlMpHUItl> U K A K U 4 I M O ct a C T ir ill i l WtUdi C: VMuMLTMXVftour >ra:i . p r o \ l h i c P M U 4 X f a k UM M O ct a* 19 KUtU: M l O c 3 00:01:10 1 it iro n (cu t MM l 10199*012 2 19199901) ) 191*99014 4 1919990IS S 101999014 101999019 10199*919 9 10199901 101*99030 10 101*99031 11 101**9022 12 101*9*03) 1) 101*9993 14 101***039 IS 101**9020 l i 101**902? 2? 101**903 19 10199*039 19 11**0)0 30 101*9*0)1 21 101**90)3 23 1019**01) 3) 1019*90)4 34 10199901S as 101*990)4 2 1019990)7 3? 101*990)9 29 10199*03* 3* 1019**040 10 101999041 31 101999042 12 101*99043 33 101*99044 14 101*9*045 IS 101*9904 ) 10199904? IT 1019**041 1 1019*9049 19 1019*9050 40 101999051 41 1019**052 Z 101*99011 4) 101*9*054 4 1019*9015 45 1019*9054 4T 1019*905 1019*9059 49 101999000 11 10199*002 52 10199*00) 5) 101999904 5 10199*005 SO 1019990? M PllU K t HUGH Blank 14CM Blank MtCM Blank T C x u s -a a sio i') -h: ; a ia n k -ii. s ic r c .r u i - a w : ::* -S.-b Blank-11. SCI T c;:u s-* T * m -Sara Blank-11. SCO TCX145-KTS101r 2It: Blank-12. SBC TC>::4S-aasi3:'.* ,? a -ll. SKC T c :::is -M S i:r -:.* .p b -ii. sex Tc?:;4S-a**io::- :- ^ p b - u . te T c ;::i!-as s io : : .; p b - U . SCO toxios-aasioi*) -i))p p b -u . i n tOX145-aaS10159 : 9 b - U . BBB *OX145-IU)S101' -SCippb-ll. BBS Toxi45-aasioi5i -?&)ppt>-ll. s u roxi4s-aaaioi> ) -19)0ppM-U. SU M?M Blank TOX145-BTS. 9R9K13M. Dyl. Contrai. *10/19/9* H I tcx iis- cts. 9*1)211. Dyl. C d a tra i.-10/19/9 f l u TO145-BTS. 933)2)214. Dyl. C ontrol,-10/19/99 M l TOXUS-MTS. 990)2)1. Dyl. C M tral. -30/1*/* I D *CXl5-ns. *R9)3)4M. Dyl, C ontrol.-lfi/19/ J O tc:u 4 S -aasm f> -2!0ppto-CCV-U-l, * t t n *C H Blank t c : i s - r s . 9*::i:SM. Dr4. Control.-10/19/** SU tc ..i4 s -a rs . 9?jj12i . or*. C o n tro l.-14/19/99 SU TC"U9-ars. sr : :i::? . or. C ontrol.- 1 0 / 1 9 / 9 SU t c . : i 4 S - a r 5 . 9.-::>?:?. Oy. C ontrol.-10/1/ SU tc::: s - bts. *?:: Pyi, C o n tro l.-10/19/ SU te ::: t s - u s i o : 2: ppb-CCV-ll-2. see H *2H Blank Tc:<i45-arsiai' :-;ppt-RS-U. 10/19/99 s u TC: i45-aTS10i:- :;:epfr-D -u. io / if /9 * m tc:::4S-ts. :1: l.'. Dyl. s no/kfl 10/19/99 s u tc:::s- bts. * : i Dyl. 5 Mj/ko 10/19/99 SU Tc :: 5 -rrs, 9;.i2;?Ji. Dyl. s a/kn 10/19/99 SU re h s - bbsiol' . :: :p p b - c c v - u - ) . s u *u : h Blank TT :45-TS. 9: 1:;:K . Dyl. s OQ/X0 10/19/99 111 TT . *S- UTS- :i}H. Dyl. 5 ne/kp 10/19/99 BBS r r : : i s - a r s . *: :i :< :m. Dy4. 5 no/ho 10/19/ BBB t: ::5-ars. :i Dy4. 5 a/kp 10/19/99 SBC r ; ;5-ts. s* :) Dy4. 5 np/kp 10/19/99 SU T- .: 5 - bsio: . :- :? p b -c c v -u -4 . see K. Blank Oy. 5 m q / k q 10/19/99 SIS TT -.5-RTS. ' Dy. 5 np/kp 10/19/99 s u T* 45- BBS1C1, : .p p o - tt v - ii- i . sib M. lank s : ) Blana-11. s u tc:.:;5 -m s ic :- - Tt:a Blank-11, SSB Tc :: 5 -tsic: C.ro Blank-11. SSB TT ;; s - a r s i o : Z Blank-1). SIB T. :.i5 -a sv :; :to-U. SSB TT :i5 -aasio : : Tb-tt. i s s V .15-R9S10: : ;p b - u . see TT. :; s - i u s i o :. s : ; s b - u . s u : . :p p b - n . see t . .is-assio:.- :s)ppb-u. t u T. ::s-* * sio : 5 :;p p b - n . see ' : 'ppb-11. i n to: ::5-a5io: -- 1 )4ppb-tl. SBC Ty Standard Standard standard i t --Bord Standard Standard Standard Standard Standard OC oc oc oc oc Standard Standard Standard Standard Standard Standard Standard Standard Standard Btd. Oane 0.9) 9.7? 24.00 49.30 9?.70 240.00 493.M 7)0.00 f??.*0 341.00 240.00 240.00 240.00 249.00 wt 7 .0 )0 7.100 7.15) 7.1)3 7.9)9 7.922 7.9)4 7.109 7 . SI) 7.110 7.002 7.14 7 .OU 7.B09 7.114 7 .1 1 ) 7.177 7.1)0 7.1)4 7.000 7.0)2 7.S3? 7.112 7.S54 7 .ISO 7.117 7.912 7.959 7.452 7 . CO 7.154 7.7B9 7. SO) 7.791 7.790 7.14 7.909 7 .IBI 7.05 7.791 7 . aio 7.B04 7.71* 7.114 7.15 7.91) 7.792 7.911 7.95? 7.BS1 4.9) 9.7? 24.90 49.30 7.70 249.00 91.00 730.00 977.00 7.914 7.113 7.911 7.B13 7.105 7.113 7.7*1 7.700 7.911 t m Finca 3725 m 5)9 SM 294 MI 171 MB 154 MI 159 m 145 4M 1074 BM 20)C MI 519 BM 515 MM 10241 mm 490? HI 10S>9 MI 117401 MM 14S235 MB 993 MM 303 MB 330 BM 14? MI 150 BM 143 MI 4*441 MI 312 MI ics m 119 MI 107 MM 14 0 m 1)0 MM 4U4S MM 315 MM 40011 MI 52BB1 MB 53155 MI 7504 MI 51114 dd 49904 MB m BM 070)2 db 55570 MI I W MOnr 13.20 2.2 1.00 0.45 0.14 0.) 0.3Z 4.90 1 9.7 -0 25.54 ) 47.10 -4 90.09 347.05 -0 501.11 2 SIS.04 -20 744.I l -2* 4. SS 1.41 a. 30 244.4? 1.15 -1 0.41 0.)2 107 MM 15)3)4 MB 705.23 22 S o a p 39119: g u n a t l l : d u d pr. -.ta: b y la 10/1/* - m e one r s s a s s s ! ; t ; t i t i E s s s s s s s s s s r sees. IP iil^ i|g !ig 8 iiii|g ||g g iii|ii|i;ig |iiS ||g |;iig g iB ii;iiiii|(i(i ! 1 l l l i I j*fp p M jI^ iif.lfJSlUi..srH. i . r . r - r . h S S S S S**??* f p 'JS p l f m V S S " m tim t ` - z n K-i, fimn;; ??mis jke m mQm mf e r " h ih i m= 51!r*M?==; 333* ` i I ..5 s 3 SMMsi ji" * '1 BS3S3 333 s 1 1 m n gaggi ss ik i r iI ss s S I I s tiiiffiU tit t- a H M#*M `` HHMH* M M I - -4 -4 # <4MW ow bw m o & fSSSS* f m s m m m m m f m m m ? B H N 0O O 6D 0 1 i HMNU i i i rauii-M 1rt, 4Uy k t. I <* - !/!/ Ot u M t i r e a U k * t i i t p M t T O i l-rtt * r 1 < . . ta /!*/** 02oup t t : u a t l i i as tor ti K /ll/tl OttM iirr C a lI ta M l lu ore TO U U -rit i r , 4*r 1 4, C M cnl * lM - A . H /U /M M o ** O M ttlfU M l 4b4 |.r lM 4 *jr l a m l l / l ) / l l OwMUiCjr CelUereetw porc ____ ie *a -r*e M t i , i i y 1 t t , k m ! <- K . X I / i l / H * * map OlUIti ad crlat4 t>r laa U /lt/M KS eooo l|i& t. I iu :h : ! iiU : L *it rc C srpc .r.l. tr.r.tK i c . `.: A S S fr **Z dec 2. : : ? fO S <( v;*d O c t 2 ;gp -e*c.proM M th aan em tb . U :4 I IM I i l l ) . SJ l f f C e t : .r. : * I :* : . r-.. O ci.'.i.-.C e:.- x i S : n i* r ;j: M r * ? :*'.** 0 ir r*<-, * s o r . : i s i r v r* -05 (C U ) . 3C zac. K . .000000 ..O O O fO O .0 0 0 . .0 0 0 0 0 O iM blwO * ' Tiw* A *` ; : HT a - nr.; T ire . ir .-s 9*< t . t i l j c r . . 1 3 i. .:to . .c a ci .4 1 1 B abid O A M bi rese a:r:-*s- " T* . < tn u 4 1 fl 1 P : yr. T-," P c:-:: : . C ::?:.-.; i i r-.::-.;: *"`a Od : 1 1 - ?*>. i - r ' . i v M ir:.; / r Mu.-;_ i - . . ** * --. J e .: a. ju - si : ' -* ; O r .. - - , ; . r O c:1' ' . . . St; .. '. . . . ' u . . A t/:' : .. - a * :* : . '-:. A t .: : - ;-! 1M U rte lu<J fX znt - *..00 ::.o o c: . 00 3 .00 ..S 3 . .00. .O C . .3 3 . O i*A id O iatold O iM bU di O m M wJ ! Q 13s - U S 3 a s u 3 3* Se E S S 0 0 9 0 E os s9 ra> 34 r. ?, S* ils ! l m ff sK U s ii ^ e ; . , s .. A ri ?- 5 P ' - ; ! ; -i " V. 1V i" ' a S S s s t i ' i i is k s 1 " r T. : ` , ` : fi 1 i T * * 1 & t 233? lili id O Q O n o ve e o Cer p r i - -*. cet j: 1*9*C \SU SS LY : i p T t t i .pro UMUnv l o m t k . db i ; :s <cn- '4*1 C e t 2: 1 0 .5 1 1 Ce.- lr.: . : < * ' c . Co - e t .'- . n j j r d ; nr V :* * * T z z e lr : ? r--- F s e te r. Q -.. I T j . . ... ;-. * l im ie r * : : s (CPA) !So m ] 1C i . oomoo. : . 009000 ;.o o o .0 4 0 0 0 su i* t d : HT T ;- . -- . - . J ' ' .* - . . . ? ; : i:r.: -.H 2 , . 030, No m ) .1 2 1 uU )ld D lU b llO CM C P y J : : - * Pe ; { (M l .ru t P c . .- A ix i l : V - : P c :..: c : ' f it 4 i:-,\:.r T A i:: - * *. : r r t ; : n .iM tf i/X MC Or - * P. r ... S rs : eV -.sd: -"r.bl4 je . . :-r* sy .= :3 . P<_. r - * U . . ; : . ; : P.H t --- 0 .0 0 1 0 .0 0 ` .00 D: - t D* " i Si . : . r.= -- . 3 .0 0 Ji* b l* 4 ;o .o o * A! Pe A i -.1 -.5 0 . .0 0 . '. 00. . 0 0 , O i * b l d O iitb lK i 0 1 a b l 4 O i * b l d / Quattro II, #64J4E SOUP 020199: FACT Equipment Log 99092 PAGE 1A ANALYST:mmh STUDY NUMBER: TOX145 MATRIX: QUSIlLDESCRIPTIONJtoli FACT Method: ETS:fclJ Injection volume:JLLuL_ __ Cycle time:JjnilL Electrode: Z-Scrrav_____ Mobile Phase: (A)2.0 mM NH4CH3CQ2 (B)JvjiQH-------- TN-A- or stndrd number (A) 9908S-10-14______ (B)TN-A:299Z- Prepared (date/by): (A )JS S im n u a h _______ (B )jfl fi2 2 ja Expires: (A) 04/00_____________ (B).,2Qie-------- Store at room temp? @ or N Other______________________ Guard column: None________________ Part number: na________ Lot number:_Qa. Analytical column. Keystone Betasil ----------------------------------------- Size: 2 x 50 mm_______________ Type:_Cl__________ Sphere sizc:JLuin--------- Part number 055-701-2_________ Lot number P9EII Serial number:0S91804Z Analytical parameters: Drying gas (L/hr); 350 ESI nebulizing gas (L/hr).13...... Sheath gas (L/hr)J2-----LC Row rale: 300 uL/min. Back pressure: 65 bar HPLC solvent gradient: 10min-10-95 Timsimnd------V J W ________ 2) _U2Q_____ 3 ) 15Q , -- 4 ) 7.50 5IM Q __________ iLL JM .210 21fi_ JLJL T u n in g M ethod R e p o rt Method: C: \MASSr.raX\SOOP-RATS.PRO\ACOODB\PFOS3 Printed: Tuo Oct X9 15:40:03 1999 Peg 1 MS SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. MS2 Set Rdbk 3.00 40 5 0.2 150 250 3.01 -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 KS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Set 14.0 14.0 0.9 0.0 4 650 Set Rd 14.0 14.0 10 2.0 0.0 40 0 650 8 38 1 f OuiuMl N r e t Dm bear Dm 11 (S*cl C oll tMrtfy (V| Co m < V i Is Is Is i 1s s Sis- :I! ! fi=s 5s hi !! f I? I S3 S "O oS sS-l s I <** I * --- s I '1 - ! iiiiI i-i"fIs ] - i " -4 M I i > -- - i f i fhi ;l lili! it SSb 2 :I I <-K I i'ijj W u I* hu MMI t Nl -3" |!-l I MN HsMi Mi sS i Mastiynx - Sample Ust Sample Ust: C:\MASSLYNX\soup-rats-pro\SampleDB\101999b.SPl.' Printed: Tue Oct 19 15:42:35 1999 Page 1 Page Position: (1,1) Pile Name File Text MS File 1 101999012 MeOH Blank 10M IN-PFOS-POAA-PFOSA-IS 2 101999013 MeOH Blank 10M IN-PFOS-PO AA-PFO SA-IS 3 101999014 MeOH Blank 10M IN-PFOS-PO AA-PFO SA-IS 4 101999015 TOX14S-RBS10199-H2O Blank-11. SEE 10M IN-PFOS-PO AA-PFO SA-IS 5 101999016 TOX145-RBS10199-Sera Blank-11. SEE 10M IN-PFOS-PO AA-PFO SA-IS 6 101999017 TOX145-RTS10199-Sera Blank-11, SEE 10M IN-PFOS-PO AA-PFO SA-IS 7 101999018 TOX145-RTS10199-Sera Blank-12, SEE 1OM IN-PFOS-POAA-PFOSA-IS a 101999019 TOX145-RBS10199-5ppt>-11, SEE 10M IN-PFOS-PO AA-PFO SA-IS 9 101999020 TOX145-R8S10199-10ppb-11, SEE 10M IN-PFOS-PO AA-PFO SA-IS 10 101999021 TOX145-RBS10199-25ppb-11, SEE 10M IN-PFOS-POAA-PFOSA-IS 11 101999022 TOX145-RBS10199-50ppt>*11, SEE 10M IN-PFOS-PO AA-PFO SA-IS 12 101999023 TOX145-RBS10199-100pob-11,SEE 10M IN-PFOS-POAA-PFOSA-IS 1 3 101999024 TOX145-R8S10199-250ppt>-11, SEE 10M IN-PFOS-PO AA-PFO SA-IS 1 4 101999025 TOX145-RBS10199-S00ppt>-11.SEE 10M IN-PFOS-PO AA-PFO SA-IS 15 101999026 TOX145-HBS10199-750pp6-11, SEE 10M IN-PFOS-PO AA-PFO SA-IS 1 6 101999027 TOX14S-RBSl0199-1000ppb-11, SEE 1OM IN-PFOS-POAA-PFOSA-IS 1 7 101999028 MaOH Blank 10M IN-PFOS-PO AA-PFO SA-IS 18 101999029 TOX145-RTS, 9R03230M, Dyl, Control,-1Q/19/99 SEE 1OMIN-PFOS-POAA-PFOSA-IS 1 9 101999030 TOX145-RTS, 9R03231M, Oyl, Control,-1Qrt9/99 SEE 10M IN-PFOS-POAA-PFOSA-IS 20 101999031 TOX145-RTS. 9R03232M, Dyl. Control,-1 0/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 21 101999032 TOX14S-RTS, 9R03233M, Dyl, Control,-10/19/99 SEE 1OMIN-PFOS-POAA-PFOSA-IS 22 101999033 TOX145-RTS, 9R03234M. Dyl, Control,-10/19/99 SEE 10M IN-PFOS-POAA-PFOSA-IS 2 3 101999034 TOX145-RBS10199-25OppB-CCV-11-1. SEE lO M IN-PFO S-PO AA-PFO SA-IS 2 4 101999035 MeOH Blank 10M IN-PFOS-PO AA-PFO SA-IS 2 5 101999036 TOX145-RTS, 9R0323SM, Dy4, Control,-1Q/19/99 SEE 10M IN-PFOS-POAA-PFOSA-IS 2 6 101999037 TOX145-RTS. 9R03236M, Dy4, Conlrol,-10/19/99 SEE 10M IN-PFOS-POAA-PFOSA-IS 2 7 101999038 TOX145-RTS, 9R03237M. Dy4, Control,-10/19/99 SEE 10M IN-PFOS-POAA-PFOSA-IS 2 8 101999039 TOX145-RTS, 9R03238M, Dy4, Control,-10/19/99 SEE 10M IN-PFOS-POAA-PFOSA-IS 2 9 101999040 TOX145-RTS, 9R03239M, Dy4, Control,-10/19/99 SEE 10M IN-PFOS-POAA-PFOSA-IS 3 0 101999041 TOX145-RBS10199-250ppb-CCV-11-2, SEE 10M IN-PFOS-PO AA-PFO SA-IS 31 101999042 MeOH Blank 10M IN-PFOS-PO AA-PFO SA-IS 3 2 101999043 TOX145-RTS10199-250ppb-MS-11, 10/19/99 SEE 1O M IN -P F O S -P O A A -P FO S A -IS 3 3 101999044 TOX145-RTS10199-250ppb-MSD-11, 10/19/99 SEE 1O M IN -P F O S -P O A A -P FO S A -IS 3 4 101999045 TOX145-RTS. 9R03245M, Dyl, 5 mQ/kfl 10/19/99 SEE lOMIN-PFOS-POAA-PFOSA-IS 3 5 101999046 TOX145-RTS, 9R03246M. Dyl, 5 mg/kg 10/19/99 SEE lOMIN-PFOS-POAA-PFOSA-IS 3 6 101999047 TOX145-RTS, 9R03247M, Dyl, 5 mg/kg 10/19/99 SEE 10M IN-PFOS-POAA-PFOSA-IS 3 7 101999048 TOX145-RBS10199-250ppb-CCV-11-3. SEE 10M IN-PFOS-PO AA-PFO S A-IS 3 8 101999049 MeOH Blank 1OM IN-PFOS-POAA-PFOSA-IS 3 9 101999050 TOX145-RTS. 9R03248M, Dy1, 5 mg/kg 10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 4 0 101999051 TOX145-RTS. 9R03249M, Dyl, 5 mg/kg 10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 4 1 101999052 TOX145-RTS, 9R03250M. Dy4, 5 mg/kg 1Q/19/B9 SEE 10M IN-PFOS-POAA-PFOSA-IS 4 2 101999053 TOX145-RTS, BR03251M, Dy4, 5 mg/kg 10/19/99 SEE 10M IN-PFOS-POAA-PFOSA-IS 4 3 101999054 TOX145-RTS, 9R03252M, Dy4,5 mg/kg 10/19/99 SEE 10MIN-PFOS-POAA-PFOSA-IS 4 4 101999055 TOX145-RBS10199-250ppb-CCV-11-4, SEE 10M IN-PFOS-PO AA-PFO SA-IS 4 5 101999056 MeOH Blank lO M IN-PFOS-PO AA-PFO SA-IS 4 6 101999057 TOX145-RTS. 9R03254-1M, Dy4, 5 mg/kg 10/19/99 SEE 10M IN-PFOS-PO AA-PFOSA-IS 4 7 101999058 TOX145-RTS, 9R03254-2M, Dy4, 5 mg/kg 10/19/99 SEE 10M IN-PFOS-POAA-PFOSA-IS 4 8 101999059 TQX145-R8S10199-250ppb-CCV-11-1, SEE 10M IN-PFOS-PO AA-PFO SA-IS 4 9 101999060 MeOH Blank 10M 1N-PFOS-POAA-PFOSA-IS 5 0 101999061 TOX145-RBS10199-H2O Blank-11, SEE 10M IN-PFOS-PO AA-PFO SA-IS 51 101999062 TOX145-RBS10199-Sera Blank-11, SEE 10M IN-PFOS-PO AA-PFO SA-IS 5 2 101999063 TOX145-RTS10199-Sera Blank-11, SEE 10M IN-PFOS-PO AA-PFO SA-IS 5 3 101999064 TOX145-RTS10199-Sara Blank-12, SEE 10M IN-PFOS-PO AA-PFO SA-IS 5 4 101999065 TOX145-R8S10199-5ppt>-11, SEE 10M IN-PFOS-PO AA-PFO SA-IS 5 5 101999066 TOX145-RBS10199-10ppt>-11, SEE 10M IN-PFOS-PO AA-PFO SA-IS 5 6 101999067 TOX145-R8S10199-25ppb-11, SEE 10M IN-PFOS-PO AA-PFO SA-IS 5 7 101999068 TOX145-RBS10199-S0ppb-11, SEE 10M IN-PFOS-PO AA-PFO SA-IS 5 8 101999069 TOX145-R8S10199-100ppb-11, SEE lO M IN-PFOS-PO AA-PFO SA-IS 5 9 101999070 TOX145-RBS10199-250ppb-11, SEE 10M IN-PFOS-PO AA-PFO SA-IS Masslynx - Sample List Sample Ust: C:\MASSLYNX\soup-rats.prtASampleDB\10199Sb.SPL Printed: Tue Oct 19 15:42:35 1999 Inlet File Bottle Inject Volume Sample Type Cone A 1 10min-10-95 91 2 10min-10-95 91 3 10min-10-95 91 4 10min-10-95 1 5 10mtn-10-95 2 6 10min-10-95 3 7 lOmtn-10-95 4 8 10mit>10-95 5 9 10min-10-95 6 10 IOmin-10-95 7 11 10ml<v10-95 8 12 10min-10-95 9 13 10min-10-95 10 14 10tnin-10-95 11 IS 10min-10-95 12 16 10min-10-95 13 17 IOfriin-10-95 92 18 IOmin-10-95 14 19 10min-10-95 15 20 10min-10-95 16 21 10mirt-10-95 17 22 IOmin-10-95 18 23 10min-10-95 41 24 10min-10-95 92 25 10min-10-95 19 26 10min-10-95 20 27 10min-10-95 21 28 10min-10-95 22 29 10min-10-95 23 30 10min-10-95 42 31 10min-10-95 92 32 10min-10-95 24 33 10mirv10-95 25 34 10min-10-95 26 35 IOmin-10-95 27 36 10min-H>-95 28 37 10min-10-95 43 38 10min-10-95 93 39 10min-10-95 29 40 10min-10-95 30 41 IOmin-10-95 31 42 10min-1O-95 32 43 10min-1CP95 33 44 10mir>-10-95 44 45 10min-10-95 93 46 IOmin-10-95 34 47 10min-10-95 35 48 IOmin-10-95 41 49 IOmin-10-95 93 50 IOmin-10-95 1 51 10min-10-95 2 52 10min-10-B5 3 53 IOmin-10-95 4 54 10min-10-95 5 55 IOmin-10-95 6 56 10min-10-95 7 57 IOmin-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 -- -- -- ---- -- ---- -- -- -- ---- -- --* -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -------- -- -- ~ -- -- -- -- -- -- -- -- -- -- --- -- Page Z Page Position: (2,1) Maaslynx - Sample Uat Sample List: C:\MASSLYNX\soup-rats.pfo\SampleDB\101999b.SPl' Printed: Tue O c t1 9 15:42:35 1999 Page 3 Paga Position; (1 , 2) File Name FU eText 60 101999071 TO X145-RBS10199-500ppt>-11, SEE 61 101999072 TOX145-R8S10199-75Qpp*>-11, SEE 62 101999073 TOX145-RBS10199-1000ppb-1 1, SEE MS Rie 10M IN-PFOS-PQ AA-PFO SA-IS 10M IN-PFO S-PO AA-PFO SA-IS 10M IN-PFOS-PO AA-PFO SA-IS Masslynx - Sampla Us! Sample U s t C:\MASSLYNX\soup-rats.pro'iSampleDB\101999b.SPL' Printed: Tue Oct 13 15:42:35 1399 Intet File Bottle Inject Volume Sample Type Cone A 60 10mfai-10-95 11 61 10mift-10-95 12 62 10min-10-95 13 10 -- 10 -- 10 -- -- -- -- Pages Page Position: (2, 2) F A C T : D A T A R E V IE W S U M M A R Y F O R M Date: f/te /ff Data A nalyst It:FA C T Study Matrix/Timepoinla: jZjiim. - 'aJ f Y . oJ" Data Review Sipt-OfT Analyit Review Name/Dale: J ac Technical Review Name/Date: / W tf ? > * & ? /< ? { Sampk List Set-up Analysis D ate/A nalyst In stru m en t: />**#*. //tt/fi *<. AhJlL Qi*vn A nalyte;. ?O & U l ) {Acceptable U n c u U nge: _ J L < _ MILO _____________ /MrR "2: _____________ j/AE xtraction B lank: Matrix Blank: t4AC alibration Choclea: M S/M SD: D ata Statua: t n i trUsi Dzl t n W ^ A nalyte: 7FS CcH*j 7-3 r*LA cceptable L inear R ange: '""~r Quality Aaninace Review Nam e/Date____________ D a ta Ennr . enlifuA__ n u - L jccaiaT - lie Ccnmcnta / Juatlfkitioaa: ^ 7 HAS A* 0u.ru*. fur- U/jL._________ Tfce S*-~t L J*r TaAAr . ~}XJa . IS U*Ja/ -Ar Orte.fu*JsAnd nJoJlAK -b**s kJ tteC. M a. %LjJ M L iM. OtLr 4'fi^fJL_kxrc SeJUX/*- 4U 7 W C r o c e a / 6 l~ jJ U I W i f i j M - __ -- '3 * r s i* /* r /n Ci/ita*'- rLtsJry TT&________ Ja,/*/. J-T' va Sr^JrcJJ '{aj- L O Q :. \R~2: Q.f?S-91> 4 MC alibration C hecks: E xtracted Blank: Irto A t * 0 M atrix Blink; A - tOQ lu tc j/a r-s b j A y A l/r l/f < 1 4 M <4 suStt-&pPAL. /c. 7 ^ 5 *./ ^ P i n i , g .r u tJ u ,* KXr*. MS/MSD: kVgjU Vo rt n ftlyA . D ata Status: ia i ,ip/ a i h i J f t n i d A "PrlH*Jc- <?t y^r a j / a y -Xsyi / T a SAju a , U L m - A n aly te: 7 f c 5 4 CCff'^ jAcccptablc Linear Range: Z-tl, i f 3 ^ 1|LO Q : --------------- Fxtracted Blank: fa* -fLa+J/lQ. R-2: M atrix Blank: 'M++-L& _ (Calibration C hecks: 4 M MS/MSD:-- ti.U y>.,,,,,,,KAflJflU,____ -7 UC lo h ifa D alaSatua: VA *" "" * " ' LM ) G o r s -r * 7& ............................ n< 1 ------------1 / C u rve j t f f t u s -fw 3>* J tv tg j- lq * - J 7 AJAS A 4u lowtr borJi s. AL/ ~H~*-_ Uaa4 L J J Z c /< m s ^-- A t .O d i. Jut M U 1J " H a . ta k .tft' J ^ 3 ` or tu*. tAJHK- u. 4 s r o /t.r' A- -AtL. /~ 7 rs *^&&f *' / } *>/ , .yi , i Ver -r? * tr a a >j* l <? & tpT -, /? % $ - i /~ > s ~ / 9 . (?) I W cvid K incljjtP A . t x l r c c M t U iiA q IT itl { K in trC e i ' Ird Curre r ilni- L'y'. AVie, tKt, H CCVv tx4rcc4cA IKo'C JCioA: OucIau. pi1 brlcJt'kva Cuve ., . C dlia'x n a ta Vtn(lu Cone 0 uc uim - FACT: DATA REVIEWSUMMARY FORM Otta Antlyav. FACT Study *: U s ___________________________-- " f o t t i ? ---------------------- --- - -- --- Matiw/Tiitu^iamts: .iky ^ * 4 j H ^ l . s_*.u / . W V ___________________ SST Inttrum enc '- A f r * - - Au-ks. niz-fiL AnaW te: C tsf HAA ceecfablc in c a r R a n a e : L O O /f* E xtriclion B lanlc / / A R A2: A i M atrix Blanlc /eA Calibration C h cck a / / A M S/M SD: ---- D tU Status: D ata Review Sign-OfT A n ely tt Review H e m e /D e le : "i*s W tsn l_________ Technical Review . . Hamc/Datc: & t,Hr To Quality A n xru ce Review N am e/D ate____________ j l 1*3 Data Entry _ J ic L ( ir tA - Y lA 4 o rC tM alja. (JC Comment]/ Juetlflcarioni: _____________________ lO/js/t @ O L 'j* * keL_.<3fig-, A f i ,. **- '& Z Z 2 . s L j / X tAAXsli J J & %- f f e j p L , . <Ce/ P` f c - J ji____ Aw'*K...P9 _pe^e- /In s ta i 4*______ j r a SJt irf <( ji f t K lq J J s V e . J t f 1L - i U S t u tJ j g J . "%* C J d t c i s - L / J ", j> r > o M ly d t s A - h Ja J J _ s a jy L ,----- tMy* ioJ ? 3eCA- . -- o-e*. C * * - J * L j J 0 * * * J c* Jl IK . Mb. C*_wi it jJ tc J c .t .'%U-ayfae J ,L L * i lx** kJ esS vjk J *>r i 3S. '& * ?/* * /? ? . s L j J b f e r * * - . r * * -y ltr C j J tie. J * "t* , - f u l J le / e J u J u . TU 5sj~*les Oye hreu-Lt-bJ Lu Me. CtcyirCS. Tr a f'. k U j (5 ) c J c U deO tdiK S iixyw '/L a U c id d lu x * r e s d j j d/bt*~ je e k . a / S o w e it. j<l/ _______ dre. (u.Js L i o.JC?), u < JL / f o ! cc l ; V' vi m \ n * I i- ic !5E r> i in I 121 i * sise mMSA KNWMBIWitttHf1i aHS n` S? S* -7 -2 :e: e fl ? H K H t i i l ii'ii iiiiii iii'iiiiiiiii ; ssiS S sS stsS se kss 3SSS sH ssSSH ss s s s s s s s s s s s s i ibisb sb ssb s s k s s s s s s s s s m s s s s s see# m s s s g g g m m if K a s s s s - s L - ss s a i s i s s s i i s i t u i s i . a. f i I 0*NP1 liS im 33322S 228S S S 2228l .f l t N N o > ir i> 4 0 '* M * n n D e > * iO '< N 9 o o n p o M fi H ooenv*oe t*e *e {**>en**a"n>#<**'< ^^ona e o o9os<g 3S2ggJ S S #** #>#*>****>* a bSyto9ta9la*MiUMMti 111111111 is :i 1i ati -sits; *i: }i l il/oi Io 0 3 tl6 il a* 1 583 8 ! sis! i i S3 a 3 3 a | ] f I fil as ^g g sS - *I*HM>M4 .N>NN. riMrirIiH I- litftftftl 35383 illi OOOOO Ititi 3i3 jm lS 8 iS i i i i " iii" . li ill >>i3>ai>ty f>.*>*>|aI OUU B***aLmimuBBHB --I (N t iiirp ii i is i ra 252| m 22222 h! iitiiiiii 1 oooooeooooeo I f SS*3 f f fS I SSeSoSaooeSo a|s|33s|fs|l||| liliiiiiiiiiiiiliiiiiilliiiiililiiiiiiiiii __ ... . o g cisb a0 b as o o o e9 f9 ao o ao 9 40999eo*o N NN N M nH H NN nN ftt'tM nftN itN N N M M K N 'tN N rtFtnN l'inrtrtetr ..,,rM M NNIlt<NNniMnlnMNN*IMI,irn'l'M >,tMMMI4NNnninilNM Ho o o a o o o o o o o o o a o o o o e o o o o e o o o o o o o a o o o o o o o e o i 5TTS27*" * ? T STSSiS S lU S 2 2 S S iS S S S IIl m m ms s s s is s ip p s s u s ts s s s s fis s s s s s s ; -- - "- - ----"'' - - - - - - - - a s S g j j s g 3 5 5 2 3 ; 2 3 | ! ! | = 5 | | 5s^s s s sgsssss f i l i n s ! M &82H2HSSS53S53sM .M M "^ s e i I i ! 3 S 3 e i OOOOODOOOOOOC ifi s o Q o o e e o o o o o o s o P O A O o t t *D*WOWo Uo Wo eUaUsWo Wo QWOWkoiMo oMO*4DM&OMPMo Wa oMsMo M MoMo aoo>Me eOoOQOOOaoOpOfiOo HHMUUUUHUUHHHUHHUMi % ssisssssIsssleEgsEEglii 222222222222 SSS* S s is s s 222222222222 3 ???????????? " -- - - - -tS-S-sbI siiss ---- ???????????? - - - TIB 'vIJMNM' ff(TJ n i f i A Hr**. PMMWIK *T*yC gS5B5SS85??g |Jin Tilill SR i S ` SSSBS fl*f * ' " 8.......... ""S8 8 898. 88??? f S ! ! sessi HR sssv s 5SSS i!liS lE J 22 f i 'i i 9 l I" BS f? Is Ma s Sit-, *1 H ,Ss3cT.s-S3c ss oeSoSSoo ssss 5 w V M o a H a a M * * S S mS S S S S o S m M< a * * a a aM6 go ua oa ru >a *a ao o< vi aav u F - H '- t ' - O e O D O O r * 0 0 0 > , aaff>*<>ao sm m m s OOOOOO e e a o o a -t e o a b e o o o o a gggm s m m c tm i i w ai a> <i ai I ------- ------ -- ------------ -- ----------------- ------------- ------------------------------------------------------------------------- -- '-----7------ Quantify CUibnu t^Mt TCUSnt mnh toy l * - at. 10/t/* *U *** * [Compound 1 name: PO A A ( Ch i ) Response Factor. 115.846 [Response type: External Std, Area C urve type: RF *-11- rtlatto by Im 10/2S/M O uwary G iU knU M > f n tQ X U l'ra c M n a <u u m . y 1 C - an. 1 0 / l l / t l S U Compound 2 name: PFOS (Ch2) C oefficient o f Determination: 0.995295 Calibration curve: 44.8833 * x + 108.462 Response type: External Std, Area Curve type: Linear, Origin: E xclude, W eighting: 1/x, A x is trans: N on e X Mil* 0X4M: QuMUtat4 hUbMl by iu X0/2S/M OUMtlfy cuuxiu >m IOU4S*t *MW llu tte M , My I 4 - i t . U / l t / H K t (Compound 3 name: PFOSA (C h4) ' [Coefficient o f Determination: 0.989156 Calibration curve: 164.764 * x + -232.515 Response type: External Std, Area Curve type: Linear, Origin: E xclude, W eighting: 1/x, A xis trans: N one ^3 ~ Am U. M34M: OmjiU U M hdiMMl by 4m 10/21/tt OuMury CAiibnUM **** T Q X U S - I l l M C I m I t W U C M . +*Y 1 * 4 - ( . l a / l t / t * M S iCompound 4 name: IS (Ch3) Response Factor 2692.44 Response type: External Std, Area Curve type: RF fa 4 A**H* >m UUM m 4 m at * ky Uc 10/3S/M PP**tW<r**TW( *'*O'WBOOPfOT'tO :* # j* anfOKnr ;!a3vi6*TtV*l*aTnf**t*^* 9 S i \: o lid is Ji 11 2o eJ ^l l a 1; 1. SI as 8? . 3S J! I 5= 1! 1 1: 2 2 {3 8 : it Co Jj j- jSi l5si*!. 9m js ei S*S s 8 U ( mt Sin "H?i! s * * " ICu 4 I I ilJ. l i: : 1 :1 ill K4b^ J ni i j j 3i C A , 1H11i :ll rssr: s.i r0si s* i s s--sB ill ill lllll i- 1a 01a Io* >s. oao 0 40 So o4o0o00o Jen* f l i t / thn ifto U : MttkCt 3I 3 S=g1 5 55 g ; 3 e s ;:4* ti b UKC ; o; i 38 lll 288 3Si i s i p f U t n y j. IUD4II 0CUffcHo" r* < * < * * JT 1^ # iiSS srs OKISH kss k ODDO Hii mi II 9 % i i s *. li l ai S I Si I1 13 l * eSsse008 a <n : i: || . : h US i S3 5 II i Ji f..~..ssslM .s.UssiXla.s V ` i" h las sisfs lss z i t i i UOU 33U & -l 2s .. lit 3 ffl* i^ fll i Ili23* SS" s I 9 * C -Sui S Si C33 sm 1115 a 999 aaaa I S88 a n fa = 1511 si 9 * S s; s m A M E L IA 062498: F A C T E q u ip m ent L og 99114 Quattro U , #6448E PAGE DATE: 10/22/99 ANALYST: ias STUDY NUMBER: TOX145 MATRIX: Rat sera DESCRIPTION: Day 1&4 dilutions FAC! Method: ETS-8-5.1 Injection volume: 10 uL Cycle time: 10 min. Electrode; Z-Spray Mobile Phase: fA)2.0 mM NH4CH3C02 TN-A- or stndrd number (A) 99085-10-14 Prepared (date/by): (A) 10/16/99 ah______ Expires: (A) 04/00_____________ Store at room temp? (Yj or N Other: (B ) McOH IB) TN-A-2945 fB) 10/20/99 ias (B) 04/00 Guard column: None______________ _ Part number na________ Lot number na Analytical column: Keystone B e t a s i l _________________________ Size: 2 x 5 0 mm_______________ Type: C18__________ Sphere size: Sum Part number. 055-701-2_________ Lot number. P9E11 Serial numben059l816Z Analytical parameters: D rying gas (L/hr): 300 ESI nebulizing gas (U h i) 10 LC Flow rate: 300 uL/mic. Back pressure: 62 bar Sheath gas (Uhr)_0^ HPLC solvent gradient: 10min-10-95 Time ( a m .) 1)0.00________ 2)1.00________ 3) 5.50________ 4 ) 7.50______ 5) 8.00________ %B 10.0 10.0 9 S .0 95,0 10.0 T u n in g M sthod R e p o rt Method: C :\MASSLXHX\AMELIA-RATS.PR0VACQUDB\PF0S1-6KV Printed: Fri Oct 22 09:58:58 1999 Pag 1 MS SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. Sat Rdbk 1.60 40 5 0.2 150 250 1.60 -14 -4 149 253 Pressures Analyser Vacuum Gas Cell Rdbk 1.2e-4 4.3e-3 MSI 124 Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier MS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens B Lens 9 Multiplier Sat 15.0 15.0 2.0 0.0 4 650 Set 14.0 14.0 10 2.0 0.0 40 0 650 1--MlUl M tM MfWt Ci ^ M |tlM U N I U A - U ,n . M \U G m \lM U * m i* I O U i* l> > n a j t e a t H * u t l m : MM Oct 11 #0;12:11 1H< K intani: r j Get 11 M i l l : U MlVMt Daisy 1 m u 1 ! .00 IM U N i 1 MRMf 1 Mm * M ir 1 CM* | I n te r O uM nl M Uy 4 Sen ) i spa ( k u m * i S ta t t TLea ( Hina 1 : Ind n a n ( Mm 1 : Rapanti j CRnannl Pacane DnapHtnr 0.93 0.99 0.99 10.00 1 Danil 4S4C1) Call 1M W <VJ Cn4M V | 1 413. 14. 9.30 10 1 CvacunA : 3 MRMi l 1 Mui nie 4 t * f ~ 1 I n t i r Oh m *) Onlay i1 Sen ) : Span 4 Dalton* ) j S t a t t TUm t KIM > : Cad TU ( Kin* 1 Rapaata > QufiMl Parane Onufhtar 0.03 9.00 9.0 10.90 1 Danil (Saca) Call lMry (V| Carni ( V 1 4**. *. 0.30 45 40 RiMUM i S MRMof 1 Mua K i r ( 1 ' | Zntar ctwuiul Delay 1 Saca 1 : Span ( Daltons 1 : Stare Tin ( Mina 1 : Snd Tina 1 Hina 1 : Rapanti : Chennai Parane OnufRtnr 9.0) 0.00 0.90 te .o o 1 IM U (Saca) Cell turor (nV| enne 1[ V | 1 421.W 10. 0 0.30 4 co NncUea : 4 MM a l 1 Nm i K l r 4 II* t tBCir C l u u i l Onlay I Saca ) i Span 1 Balconi ) : Scart Tina < Kinn 1 i tad TUm 1 Mina ) : Rapaata : Channel Tarant Oaoqhtar 0.03 0.90 9.0 10.00 1 Oaell (Saca) Cell tn e r y (#V) Cena { * 1 l 414.09 7. 09 9.40 43 0 1 H .tbod R eport Method Fila: Last Modified: Printed: ci\aaalynx\enlia-rate.pro\ac<iudb\10inin-ia-95 Friday, Octobar 22, 1999 0 9 iS S i36 Friday, Octobar 32, 1999 09>59>25 Page 1 HP1100 LC Pump Initial Conditiona Solvents A% B% C% D% 90.0 lo.o 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 Pump Gradient Timetable The gradient Timetable contains 5 entries which are : Time 0.00 1.00 s.so 7.50 8.00 Al 90.0 90.0 s.o 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 KP1100 LC Puap Sxtarnal Xvant Timatabl* The Timetable icontains 3 entries which are : Time Initial 0.00 0.10 Column Switch Contactl Off Off Off On Off Off Contact2 Off On Off Contacts Off Off Off Contact Off On Off HP1100 Xutoaaaplar Initial Conditions Draw Speed Eject Speed (jil/min) Draw Position (mm) Stop Time (mins) Injection Volume(//l> Vial Number 200.0 200 0.00 9.00 10.0 13 Masslynx - Sample List Sample Ust: C:\MASSLYNX\amelia-tats.PROVSampleOB\ia229fla.SPL Printed: Fri Oct 22 0 9 :5 8 : 1999 Page 1 Page Position: (1 ,1 ) File Name File Text MS File 1 102299001 MeOH Blank lOMIN-PFOS-POAA-IS-PFOSA 2 102299002 MeOH Blank 10MIN-PFOS-POAA-IS-PFOSA 3 102299003 TOX145-RBS10199-H2O Blk-12, SEE 10MIN-PFOS-POAA-IS-PFOSA 4 102299004 TOX145-RBS10199-Serum Blk-12. SEE lOMIN-PFOS-POM-IS-PFOSA 5 102299005 TOX145-RTS10199-Serum Blk-12, SEE 10MW-PFOS-POAA-IS-PFOSA 8 102299006 TOX145-RBS10199-5ppb-12, SEE lOMIN-PFOS-POAA-IS-PFOSA 7 102299007 TOX145-RBS10199-10PPP-1Z SEE 10MIN-PFOS-POAA4S-PFOSA 8 102299008 TOX145-RBS10199-25ppb-1Z SEE 10MIN-PFOS-POAA-4S-PFOSA 9 102299009 TOX145-RBS10199-50ppt>-12. SEE 10MIM-PFOS-POAA-IS-PFOSA 10 102299010 TOX145-RBS10199-100ppb-1Z SEE 10MIN-PFOS-POAA-IS-PFOSA 11 102299011 TOX145-RBS10199-250ppb-12. SEE lOMIN-PFOS-POAA-IS-PFOSA 12 102299012 TOX145-RBS1019B-S00ppt>-12, SEE lOMIN-PFOS-POAA-IS-PFOSA 13 102299013 TOX145-RBS10198-750pp6-1Z SEE lOMIN-PFOS-POAA-IS-PFOSA 14 102299014 TQX145-RBS1019B-1000ppb-12, SEE lOMIN-PFOS-POAA-IS-PFOSA 15 102299015 MeOH Blank lOMIN-PFOS-POAA-IS-PFOSA 16 102299016 TOX145-RTS-9R03245M, Oay1.5mg/kg, 050-6x110/19/99 10MIN-PFOS-POAA-/S-PFOSA 17 102299017 TOX145-RTS-9R03246M. Day1.5mg/kg, D5frext10/19/99 lOMIN-PFOS-POAA-IS-PFOSA 16 102299018 TOX145-RTS-9R03247M, Day1. Smgikg. D50-xt1Q/19/99 lOMIN-PFOS-POAA-IS-PFOSA 19 102299019 TOX145-RTS-9R03248M. Day1. Smg/kg. 050-ext10/19i99 lOMIN-PFOS-POAA-IS-PFOSA 20 102299020 TOX145-RTS-9R03249M. Oay1. 5mg/kg. D50-ext10/19/99 lOMIN-PFOS-POAA-IS-PFOSA 21 102299021 TQX145-RBS10199-250ppb-CCV-11-1, SEE lOMIN-PFOS-POAA-IS-PFOSA 22 102299022 MeOH Blank lOMIN-PFOS-POAA-IS-PFOSA 23 102299023 TOX145-RTS-9R03250M. Day4, Smg/kg, D5O-ext10/19/99 lOMIN-PFOS-POAA-IS-PFOSA 24 102299024 TOX145-RTS-6R03251M. Day4, Smg/kg, D50-ext10/19/99 lOMIN-PFOS-POAA-IS-PFOSA 25 102299025 TOX145-RTS-9R03252M, Day4,5mg/kg, 050-6x110/19/99 lOMIN-PFOS-POAA-IS-PFOSA 26 102299026 TOX145-RTS-9R03254-1M, Oay4. Smgrtcg, 050-10/19/99 lOMIN-PFOS-POAA-IS-PFOSA 27 102299027 TOX1 45-RTS-9R03254-2M. Day4. Smg/kg, 050-10/19/99 lOMIN-PFOS-POAA-IS-PFOSA 28 102299028 TOX145-RBS10199-250ppb-CCV-11-2. SEE lOMIN-PFOS-POAA-IS-PFOSA 29 102299029 MeOH Blank lOMIN-PFOS-POAA-IS-PFOSA 30 102299030 TOX14S-RBS10199=-H2O Blk-12, SEE lOMIN-PFOS-POAA-IS-PFOSA 31 102299031 TOX145-RBS10199-Serum Blk-12. SEE lOMIN-PFOS-POAA-IS-PFOSA 32 102299032 TOX145-RTS1Q199-Sefum Blk-12. SEE lOMIN-PFOS-POAA-IS-PFOSA 33 102299033 TOX145-RBS10199-5ppb-12. SEE lOMIN-PFOS-POAA-IS-PFOSA 34 102299034 TOX145-RBS10199-10ppb-12, SEE lOMIN-PFOS-POAA-IS-PFOSA 35 102299035 TOX145-RBS10199-25ppb-12, SEE lOMIN-PFOS-POAA-IS-PFOSA 36 102299036 TOX145-RBS10199-50ppd-12. SEE lOMIN-PFOS-POAA-IS-PFOSA 37 102299037 TOX145-RBS10199-100ppb-12. SEE lOMIN-PFOS-POAA-IS-PFOSA 38 102299038 TOX145-RBS10199-250ppb-12, SEE lOMIN-PFOS-POAA-IS-PFOSA 39 102299039 TOX145-RBS10199-500ppt>-12, SEE lOMIN-PFOS-POAA-IS-PFOSA 40 102299040 TOX145-RBS10199-750ppb-1Z SEE lOMIN-PFOS-POAA-IS-PFOSA 41 102299041 TOX145-RBS10199-10Q0ppb-12, SEE lOMIN-PFOS-POAA-IS-PFOSA V 95 12 5 >99999 ) (0 (O IO (O CO t (ft (Ji o I * V r3 * O uCN<<OOK)U*4auUMM^O WN a S ao I I I I I N I I i I I N I I I I II I I I II I I I I I I I I I I I I I I I I I I ! I I I I II t I I ! Il ! Il I I I I I I I I I I I I I I I I I I I ! I II I I I I I 1 ! I ! 1 I I Il I I I I 1I I I I I I I I I I I I I I I I I I I I I I I I 8 8 Q 1 I I I I I I I I I Il I II I I I I I I I I I I I I It I I I II I I I I I II I I I II I I I I I I I I I II I I I I I I I I I I I I I I I I I I I I II I I I 8 8 1 1 I ! I I I ! I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I. I ! I ! I I I I I I I I I II I I I I I I I I I I I I I I I I I I I I I I I I I I I Oo 8 m 8 8 *0 S ? FACT: DATA REVIEW SUMMARY FORM D ate: Data A nalyst FA C T S tu d y It: Matrix/Timcpointi: / y i / S f / r - , f f k y i* Y ik /tu fo n j? ... Sample Lit Set-up Analysis D ate/A nalyst buuuraent ?7, ,-Q k / ,Q i/P 7 > -r p ^ Data Review Sign-OfT A nalyit Review N a m e / D a t e __ /tfX/ Quality A ssunse* Review Name/D ate:____________ Data E ntry:. Commenti / Justificaliona: I kh W * h 9 & /y > /___ LOQ: r ^ : (4. r fr fr f/ Extraction Blanlc A f c U f M i a B im fc */i -L>l s?}/r> V A ~ S c , /P J r -S 1? K _____________________ M S /M S D :_______________/ 0 / A ^ ' A M f iiw w . D ata Status: ( J ) $ } ^ J , ) , w , TXO l f l l j fc l/M rs/yldil JAfcJnM<ft J ? f L * ? \ @ / // o < ? r7 ra rf~ Analyte: ^ /yl//S sr~ > - O n # S Acceptable Linear Range: r f l ? - ' r f f ? ______ LOQ: r f. ? r f Extracted Blank: ^ R"2: /}. Matrix B lin lc - f / L&L k tu^2i22J J A & tf. fib p u n S - f i n y J M O / f / p C Calibration Checks: MS/MSD:______ IK - tiflVcc u n i U fe uixq.__^,l. P a ta S u tu s/jT ) WirC A aV A t i r U - (A C - S rfn t / ' / / <=? f i f i s M a n -. x r j. # '` 7?7 A n a ly tee: Acceptable L inear R ange: LOO: -- ~~ R*2: ' Calibration Chcckx: MS/MSD:_______ Data Sama: Extracted BUnk: _ Matrix BUnk: TL Z ! 'K i" >iW ua mo owomomo mo mo ho mo ho ho mo owohchmowowo ua mc ui mo u< m> m w eu*BBmBh*homomo m* na ho ho ho mD wa (I SI B t t A O O O a O O > aB O 0 0 A eeO A O 6 A a * A O A 000009000 ! "U \fo n^ ma*a lf *! - liiilliliii iliiiiiiiliiH i illlii Iiil slilssIIssiEs ................................................. : s s s ts s s s t s i : ss ss s :. . i i i i K S i i i i i" ~ - ' * H g-.................... S . --t . t *** s: " "" " 7 7 7 t n x 1S ! W N N N tftf MW _____________ lm ? * ' n n mm f f f l i ! f i i P c c f .- F ^ f g |p |||I I I s g l il li fi ?i mI lIHr . rt. e * S 5 _TC BKC- BBSSSi5a^-'8 i ? i m i 8BEBBSa,,;-:s Sfl r r ' U r a fi l SB 1 i ? s s?;s; s"s :sssss i n\\ i s slsl M mSmS * *B" B 1 lili H S SSB 5 <S SS f T I 111 ooooo Rflfifi SS [[lilil! 5SSSS s < tS S O m. O te te a Mm S W a S o ` O MO MIOO 4Wf>O OWO O0Mte ;g g sfH f K B tcg g sS sffS S S M H | uwSCSiS Sant!Sww* M H a M 0 a W k > w M a A H a * * > H w w I i j 3 - S 3 7 ': -7 T-- S31X 1:-" - CIJIMlllimimiIllIlfHIllIlllillillIllllI 3SS5=5|||||pasS|=E3S52===Ssl||| i " f f l 8 8 8 55S8H Qwwilfy Cniimiil t a n u y -Mt I U i ce Br 144 rtllwtl a^ U U lti iM t aa d lU M : Mm Occ >S U >i !* M tM : ci ut <mU(iid: tMOet Otsll'll 2*# *ri*rt N O e 2 4 l O s S l t l * 11 1 102SH 3 mstMit I imitati A1021*1043 s 1025*9041 4 l39**t44 3 1439**041 14X999440 14X9**047 14 14299*44 11 10299144* 12 102999090 13 102999491 14 10399*493 19 1039**493 10 1039**094 17 101999499 10 2039**090 1 1029**097 30 1039**49 21 1029*9099 22 142999040 21 102999001 24 102999002 29 103999403 20 102999004 37 102999005 2 1025*9000 29 101599007 20 102599000 U 1029*9009 33 10299*070 U 1429*9071 34 10291*072 35 19259**73 30 1035*9074 37 1025*9075 30 102599*70 )* 10299*477 0 1029*9070 41 10399907* 43 1025*9400 43 103591011 44 10359*002 45 1029*9401 O M u a t TW t M ao U M k IM O U ao k TOX145~UkS19l9*-OQO I t t - U . I U TOXliS-ftlSlOlOt-teru *12-12. *** TOX145-HT10!**-* *1*-13. I O n u 4 H tu u i* i> * * 0 'U < n i TQxi4S-usiai9*',i4ee>i2. m fou>usuun*iii*0'U< ** to u 4 i-iu u if* 'M f* * * u . n TOXUS-Uf1019l-l90M9b-12. SU TQX14S-USlQl*9-190Rpb-12. SU tOX145-**l01f*-5*4ppto-U. SU TDXi43-U0l019*'7J4f4b-l2. SU fQ U4SU im if<U I*0*U . SU w St lient S tw O w d SftciaodrtiefOr TOU49-RTS-9S4324SK. U y l. 9/*. 10X145-*T*-U2244lf. S w l. */*. DS0-Xtl/l/** 10X2i f - n s - 9*0324*. 0*jrl. 5-d/fc. p 5 0 - **l/l*/t* TDX245-STS-9S0124M. U y l. U / H . W O - U tl / /* * TOX145-TS-**0134**l, ta y l. ta * /M . 0 0 - tlO /l* /9 * T O X U l - M O m - l H>> c o r - u - i . S U TOH4S'W iHm-HW -U, SU QoCc M O I SIm * 1OX145-ST9-IR013S0K. Doy4. Sa/fc. O $0-xtl4/29/ff 1CX&45-n9-*03251M. 0 * Y * . 9m0/*4. P 5 0 -* e* l /l* /f* TOJU4S-CT4-9M3252X. Ocy4. S0-*fcl0/l/** TOX145-*TS-f*01254-U. Uy4. */*. D90- 10/2*/** 1QXU9-ftTS-*R#)2S4-2M. Uy4, Sag/** T441-MI101-OWI>-OW-U-. SU TQX145-**S19l9*-230pp6-U. S U TOXi4S-**Sm**-290ub-CCV-tl-l. SU TOX145-OLSm**-350pb-CCV-U-4. s u M- 24/lf/* gc QC QC QC T O X 14S-**S101f*-*3O * L * -U . S U T O * 1 4 5 -* * ftl 1 9 9 -S n *14-12 S U ro x i4 S -ftT * io i9 -S 4 u n m ilk - 1 2 , S U TO X 345-R *S1019-$U *-U . S U T 0 X l 5 -ft*S 1419-19fb-12. S U T O U 4 5 -JU tfl0 1 * -2 S p -U . S U T O X 145-U 9101f-9O ppb-12. S U T o w -u n ii i-iM p p n :. s u T O X 1 4 9 -* * S 1 0 1 * -2 S 4 |V b -t2 . S U T O X 1 4S -W S 101**-JO flppb-U . S U tO K 1 4 3 -* S S 1 4 1 9 l-7 5 4 p ti-t2 . S U T Q X lil'H JS lO lH -lO O O p p k -H . S U Sceartard Steadard itearterd Seeadard Steortr4 tceartacd IlucteMOUtrrOd JttM U ld caao 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 l.0 1.00 1.00 1.04 1.40 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 U 7.101 7.211 7.211 7.214 7.227 7.295 7.201 7.211 7.290 7 .3 7,229 7.209 7.314 7.211 7 .1 7 .2 7.211 7.171 7 . UC 7 .1 7.140 7.190 7 .1 7.119 7.074 7.093 7.074 7.09* 7.07 7.102 7. OSO 7.100 7.102 7.11* 7.090 7.101 7.0*2 7.131 7.0*2 7.09* 7.102 7.092 7.101 7.099 t u f t k ri** 14 bb 1 4 bb 2074 bb 2330 bb 3010 bb 2937 bb 3090 bb 2574 bb 3 9 bb io m u n bb 1030 bb 2041 MM 9 bb 09 bb 0 MK 71 bb 42 bb 49 bb 1905 bb 2900 bb 3 bb 47 bb 43 bb 40 bb 40 MM 95 m 1*07 M 2*31 bd 3*49 bb 2911 bb a im 3410 bb 1197 bd 2944 bd 3177 bd 3074 MK 2990 MK 2749 bb 1443 bd 143 bb 3712 bb 1771 bb 1415 m ewM. M * 0.00 -100 l.U IL 0.91 -9 0.71 -29 0.99 -3 0.91 -7 .92 t 0.S3 -14 0.94 -4 0.97 -3 1.01 1 0.94 -4 0.94 -4 0.00 -100 .2 -94 0.02 -9# 0.02 - ta 0.01 -9* 0.02 -9a 0.91 -9 0.99 -11 9.90 -100 0.02 -90 0.01 -99 0.02 -99 0.02 -9 0.02 -99 0.40 -40 0.90 -10 0.91 -7 0.93 - t 0.00 -100 1.19 15 1.00 0 0.9) -7 1.01 1 0.90 -2 0.94 -4 0.07 - I l 1.0* 9 1.0* 1.14 10 1.20 20 1.17 17 H J Soup 02010*1 4 tfM in 4 M 10/24/* guM tU y C *U br*tla papar* M m U Si l * t M r t , Bay I M t t t a U w * M A / w* i a m m asta! O u a tiu ftnwily MUwmIw Hitgitirr tM u s t i u a 144 t t i n i u , a n w / M / M , > 3 4op OlOlHi QMMlUt Ml prit* Br SCltt u m U IM H tClMH kr h if/se/M fA im o ooo O o' V V * aaa SI i i js lili Haetaod Mporc Kathod CU: Laac *oitl4: COHPOWM4. Pria* Ci UUSSlYia\oup4a0191 .KV**chttU02999b.ab tu Oec 2 4*UH 1999 I . POSA Tu# oct J4 19s*J>l<t 19*9 C--BUbd Ma**; U tU M l ti( - l Q iu iflty Trse: Cooc. * ItM Bnlai DHr T Valu; Dmc Nk f a e t a n ninw fetr: OwcMUfr* a u winOin POSA (MM) TIC Ceac. > 1.040090. OiMblad 1.040040 2.440 1.40400 M tH C iw Ta (!) I M a ti v * IMUMita Tlaoi ST U f t r u c * ; T1m# Wiodow (**) i HX SlCCiOtt; 9.944, 0.444. (MM) 0.444 ftabl4 oiabld OMTMt iMpMMfi te m l A Pelyw miil TV*: In t o t Ocilni r i e weiebtiaet Ajci# TrM(OMlCiM: Otai C#j U aur feaeluda l/i Nom HlfC>{Mk tapUtUd: Onathla#; WiatfOU is (CA)! Muobar etc --nnenas Wwotblng Mtliedi Jo ta **ll*y tlUMMlddue# p#A caiximrt Soi b#11 i-----1------- Dr tbr#bald; 0cct taoulSAr: Sbouldor Chxateld: ooblad 2 1 )0.44 244.00 S. 44 90.00 Oibld 14.04 Sloti taaiehe: Abeeiuc baieOt: M U d n jt: Abelac ci 1.90. 4.44. 2.40. 4.44. D1m M4 O iuU l Diatald DiaabUO : i im 1153 _ aoo o v*reic 2 eiu-*feol4: re houli*-*: 33 a I 31 * Wa * Wa e31 S ilii Quattro II, K414E SOUP 020199: FACT Equipment Log 99092 PAGE 1/1 DATE: 10,25:22 ANALYST :mmmh ___ STUDY NUMBER: TOXI4S MATRIX: E iU ^D ESC R im O N JM U iflD i FACT Method: ETS-8-5,1 Injection volume: 10 uL Cycle time:, IQjnin, ElectrodetiSiaai------ Mobile Phase: <A12.0 mM NH4CH3C02 (Bj.Msg H------- TN-A- or stndrd number (A) 99085-11-3_______ (B) TN-A-2997 Prepared (date/by): (Al 10/21/99 tnmh (B) 1/1&99 ah . Expires: (Al 04/00_______ (B)_2sue_____ Store at room temp? @ or N Other:. Guard column: None________________ Part number: na________ Lot number:jta Analytical column: Keystone Betasil________________________________ Size: 2 x 5 0 mm______________ Type:_Q__________ Sphere size:J j m -------Part number: 055-701-2_________ Lot number P9E11 Serial numberflfiJlSSSZ. Analytical param eters: Drying gas dJluT. 350 ESI nebulizing gas (LVhr)JJS___ Shealh gas (L/hr).Q. LC Flow rate: 300 uL/min. Back pressure: 65 bar HPLC solvent gradient: 10min-10-95 Tim e (m in .l DM2_______ 2UQ _________. 3 1 5.50 417.50 5UL22__________ 33- JM . JLiLSL J212. 212- I2JEL Tuning Method Report Method : C t\K\SSLYWC\SOOT-RXTS. PR0\ACaUSB\PP0S3 Printed: Mon Oct 25 16:37:32 1999 Rage 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 -SO -6 151 250 Prosurea Analyser Vacuum Gas Cell Rdbk S.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 mumu ctNnww\wwM.wauo8BBiviwni iroi-iau-w m .H t u t Ito iU lM ti f r l O ct IS U a S S ilS l ) M tv ia u li a* OR as I l t l l i U ISO* S o l H t O a ia r I a ia * ) t S .M ru c tlu t l Mot a t 1 Mum wmtx { j Xatar Ctiaaaal Dalay < Sac ) i Spaa ( Oaltaaa ) i Scare tim m ( Miaa 1 ta d TiM 1 Miaa ) i ftapoata i Q u a m I Oaroae t a u g i u r 0.0) 0.00 0.00 10.00 1 (M il (Saca) Coll Maargy <oV) Com ( V > 1 411.00 119.00 0.10 JO IS taaeclM t 1 w t 1 Maa P a ir t *- j Xatar CIi m m I DtUjr 4 Sees ) Span ( Dalcoaa ) t aauudt r Te iTwiM{ < lU him ut )i lUptit t O m o m I t n a t D sugliei aa..a 10.00 b m i i t i M d c i i saourgy <vi lvi m . M a * . so a .io 43 CO rwwctla* I 1 MM A* 1 M u* H l r ( MSP- ) Xatar f t i n u l Dalay { am ) t Spaa ( Ooltoaji > i S ta r t TiM ( Mia* I i nd TiM ( Mima > : M p o ti t OtacuMl Far at D u R M r a.ai a .a o a1.0a.o00 1 O nU (M i) C a ll aoargy UV) Co m ( V ) 4M.00 7. 00 0.10 43 40 i 1 m m air 4 N*- } Zk w Chanaa l M lty ( Saca | $ Su a ( M l t N I J I S ta r t T4m ( Miaa ) : Knd Tim < Miaa ) s U pati i Chaaaal Paroat Daughtar 0 .0 1 00 ..00 00 110.00 Dm I I ISk i ) C all Baargy <V) 0.10 40 ** Method Report 711x Uat Kodlfiad: Irihtad: ci\Maalyu\aou9<ntt.pro\eiidbU0Hia''lS-)S Monday, OcteJhar 2 5 , I f f IfiMtSI Monday, October 35, 1999 lliUUI 91100 t C rump Initial condition* Solvents A% B% c% D% 90.0 10.0 o.o 0.0 Flow (ml/min) Stop Time (mins) Min Pressure (barj Max Pressure (bar) Oven Temperature L*ft(C) Oven Temperature Right(C) 0.300 10.0 0 400 30.0 30.0 BP1100 LC Pump <3radiant Tlnatabla The gradient Timetable contains S entries which are : Time A% c% 0 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 loo ic ruap Sartaxnal Bvant Tiamtabla i 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 1100 Autosamplar Initial Conditions Draw Speed Eject Speed (ul/min) Draw Position (mm) Stop Time (mins) Injection Voluma(pl) Vial Number 200.0 200 0.00 9.00 10.0 9 ?aga 2 Pressure 400 400 400 400 400 Maialynx Sample Uai Sample List C:\MASSLYNX\soup-rals.pro\SampleDBYI02599b.SPL Printed; Mon Ocl 25 16:32:57 1999 Paga i Page Position: (1,1) File Name File Text MS File 1 102599039 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 2 102599040 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 3 102599041 TOX145-RBS10199-H2O Blk-12. SEE 10MIN-PFOS-POAA-PFOSA-IS 4 102599042 TOX145-HBS10199-Sanjm Blk-12. S S 1OMIN-PFOS-POAA-PFOSA-IS 5 102599043 TOX145-HTS10199-Semm Blk-12. SEE 1OMIN-PFOS-POAA-PFOSA-IS 6 102599044 TOX145-RBS10199-5ppb-12, SEE 1OMIN-PFOS-POAA-PFOSA-IS 7 102599045 TOX145-RBS10199-10ppb-12, SEE 1OMIN-PFOS-POAA-PFOSA-IS t 102599046 TOX145-RBS10199-25ppb-12. SEE 1OMIN-PFOS-POAA-PFOSA-IS 9 102599047 TOX145-RBS10199-50ppb-12. S S 1OMIN-PFOS-POAA-PFOSA-IS 10 102599046 TOX145-RBS10199-100ppb-12, SEE 1OMIN-PFOS-POAA-PFOSA-IS 11 102599049 TOX145-RBS10T99-250ppb-12. SEE 1OMIN-PFOS-POAA-PFOSA-IS 12 102599050 TOX145-RBS10199-500ppb-12. S S 1OMIN-PFOS-POAA-PFOSA-IS 13 102599051 TOX145-RBS10199-750ppb-12, S S 10MIN-PFOS-POAA-PFOSA-IS 14 102599052 TOX145-RBS10199-1000ppb-12. SEE 10MIN-PFOS-POAA-PFOSA-IS 15 102599053 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 16 102599054 TOX14S-RTS-9R03245M, Dayl, Srng/kg, 050^x110/19/99 1OMIN-PFOS-POAA-PFOSA-IS 17 102599055 TOX145-RTS-9R03246M. Dayl, SmofcB. 050-6X110/19/99 10MIN-PFOS-POAA-PFOSA-IS 18 102599056 TOX145-RTS-9R03247M, Oayl, SmVg, DSO-extl0/19/99 10MIN-PFOS-POAA-PFOSA-IS 19 102599057 TOX14S-RTS-9R03248M. Dayl.SmiFkfl. D5a-axMO/199 1OMIN-PFOS-POAA-PFOSA-IS 20 102599058 TOX145-RTS-9R03249M. Dayl, 5mg*0. D50-ext10/19/99 1OMIN-PFOS-POAA-PFOSA-IS 21 102599059 TOX145-RBS10199-250ppb-CCV-11-1, SEE 1OMIN-PFOS-POAA-PFOSA-IS 22 102599060 TOX145-RBS10199-250ppb-12. S S 1OMIN-PFOSPOAA-PFOSA-IS 23 102599061 MeOH Blank 10MIN-PFQS-POAA-PFOSA-IS 24 102599062 TOX145-RTS-9R03250M. 0ay4,5mg/kg, D50-ext10719/99 10MIN-PFOS-POAA-PFOSA-IS 25 102599063 TOX145-RTS-9R03251M. Day4, 5mg/kfl, D50-ext10/19/99 10MIN-PFOS-POAA-PFOSA-IS 26 102599064 TOX145-RTS-9R03252M. Day4, 5mg/kfl, D50-ext10/19/99 1OMIN-PFOS-POAA-PFOSA-IS 27 102599065 TOX145-RTS-9R03254-1M. Day4,5mo(g, D50-10/19/99 10MIN-PFOS-POAA-PFOSA-IS 28 102599066 TOX145-RTS-9R03254-2M, Day4, Smg/kfl, D50-10/19/99 10MIN-PFOS-POAA-PFOSA-IS 29 102599067 TOX145-RBS10199-250ppl>-CCV-11-2, SEE 1OMIN-PFOSPOAA-PFOSA-IS 30 102599068 TOX145-RBS10199-250ppb-12, SEE 10MIN-PFOSPOAA-PFOSA-I3 31 102599069 TOX145-RBS10199-250ppb-CCV-11-3, SEE 10MIN-PFOS-POAA-PFOSA-IS 32 102599070 TOX145-RBS10199-250ppb-CCV-11-4, SEE 10MIN-PFOS-POAA-PFOSA-IS 33 102599071 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 34 102599072 T0X145-RBS10199-H2O Blk-12. SEE 10MIN-PFOS-POAA-PFOSA-IS 35 102599073 TOX145-RBS10199-Semm Blk-12, SEE 10MIN-PFOS-POAA-PFOSA-IS 36 102599074 TOX145-RTS10199-Seium Blk-12. SEE 10M1N-PFOS-POAA-PFOSA-IS 37 102599075 TOX145-RBS10199-5ppb-12,SEE 10MIN-PFOS-POAA-PFOSA-IS 38 102599076 TOX145-RBS10199-10ppb-12, SEE 10MIN-PFOS-POAA-PFOSA-IS 39 102599077 TOX145-RBS10199-2Sppb-12, SEE 10M1N-PFOS-POAA-PFOSA-IS 40 102599078 TOX145-RBS10199-50ppb-12, SEE 10M1N-PFOS-POAA-PFOSA-IS 41 102599079 TOX145-RBS10199-10Qppb-12. S S 10MIN-PFOS-POAA-PFOSA-IS 42 102599080 TOX145-RBS10199-250ppb-12. S S 1OMIN-PFOS-POAA-PFOSA-IS 43 102599081 TOX145-RBS10199-500ppb-12. S S 10MIN-PFOS-POM-PFOSA-IS 44 102599062 TOX145-RBS10199-750ppb-12. S S 1OMIN-PFOS-POAA-PFOSA-IS 45 102599083 TOX145-RBS10199-1000ppt>-12. S E 10MIN-PFOS-POAA-PFOSA-IS Maaslynx - Sampl Llat Sample List C:\MASSLYNX\soup-rals.prolSamplaDB\102599b.SPL Printed: Mon Oct 25 18:32:57 1999 o o o o o o o o o o"*g"*o"*i' 333333333133; ??? "* J^ i 2 0 0 0 j | ^ j | ^ o o o S o o o g 3 3 3 3 | 3 | | .3 3 L .I .I .i .i .i .i .f .I |3 11.1.11. ?'?'?'? ? ? ? ? ? ? ?'? ? ? ? ? ? ? ? ? ? ? ? ? ? ? y 999 SSSi >---9---9---9--9>B99 9^ 9 s9 9 g9 g9 g9 g9 g9 g9 g9 g9 g9 g9 g9 g9 9g 9g 9g 9g 9g 9g 9g 9g 9g 9g 9gi9ugi9cin;9u&i9tgn9cg, BiigSSSgKSBISiSSafcSfciiSiSegSSfcSSgggSiSeiigaSgSaBKBRiiSS 23. & 3 I OOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOQOOO WWCOWMWMWW I ff p g p g ? ? ? s r 1 llliiilll aaaaaaaaa !' Oo nD oDnD'I ! 8 8 '' f <o c 976 4*ro<o*!0<o*| l JR & T* P .**^i<o 1 | 1 ! ISISKS' I aattta !! 1 1 !SS I 01 OB 1 1 ! 1 !|gK3feK5i to * i u i it t I i roroMNi | | | 1 t f M M I 1 t 1 | t **j * io * m e * ysisficjggyg ' ' 111 * 1 1S i ! 1 1 1 1 13 8 S S 3 i i 8 o > l I ! ! ! I I II I M I ! ! ! ! 1 ! ! 1 ! I ! I I ! I I ! I I I I I I I 1 I I ! I M I s 3 o Pa92 P*Q8 Position: (2,1) FACT: DATA REVIEW SUMMARY FORM Oste: Data Analyst: FACT Study*: ,/Z $ c h < L M atnx/Tim cpointa: & h $ Y G ? '//'.> s r j rth y / V - S / Sample Lot: , / 6 < f l 7 9 % h - . ------------------------- Set*upAnalysts Date/Aiuilyst. /O ' 7 -9 * 7 >CtX t In strum ent: A u ljitc , Acceptable L inear R in g e: "7900 ~ 9-ftp-O ___ LOO: / f - fO p lo Extraction Blank * O h C ^X R*2: / I *9*9S ^ K Malrix Blank-. J /z JL Q L . Calibration Checke /O /^ ___________________ _ ________ MS/MSD K )c J^ilCtct Va)>H\ Pp mt r DataStatu:(7)(?) EoWtA IAC- U>)niW Data Review Sign-0 fT A ealyrl Review Name /D ate: " ,/ Q k / ..,. j k h tofltltf QualityAsauranceReview Name/Date__________ DataEntry:. E-In v u i l A t l o h ' l l t ' l Canumota/ Justifleationr: ih (//fZ/Z/Z/aS <rr"J /,s/jw ' /& # ?> ^ / / / / - a u o t j L , ___________________ a x * * 9 fa p tf/S O ^vtL ro M a ^n Z & t/A S Jnvs rf/L >u*A.Uha/ J&*~ /v r fy r / n oe A j z J d tu M .________________ J b '& T ? Analytic Acceptable L inear R ange: LOO: ............... ..... R"2: Calibration Cheefcx MS/MSD: Data Status Analyte J 'tS ' Calibration Checke MS/MSD.______ D ataSattu: Extracted Blank . Matrix Blank:__ Extracted Slant _ Matrix Blant (/i//f/ 9/p /ton/snfa/z/ S rb/V7 /K/i Ouv/t/ 7dM*/c rt/srsi/u o f ty j U A /S fc . Q /7f s ita ti Z tffo/K f /far- S \ ^ 3 //J 7 /n ( ^ \ U 99i-rG eesrr> ejc ^ J s_ - J y / p / ^ s f i o ^ C. < 9 /tew fV . (r^C Q rm m o> J < M 'iejr> *J flo A > t/r//fe< k U A C ?\ . A lo ^ /r f)& *sfT r Ifj -G A +^g A * T xtoAf oe av,g //rf-q -y^s-A/ncK'/t^j-r M w i r f pu (Nnmnwtik m o to ***a SSiKSSSiiCiSSStiKSSiSSiSKSSSSSSCCrs. I liPli! j, I V M 51 i ! ! I i i if 2s=:3s - . o ssssssss: ss 3S ..O m SSSS3 ,, 3 illii S S H ia i J iiiiis n ld lH jIS fS iii ii iS i^ t ililliiSSSEiSIiliSisillllfilSSSEiSSSSSiSliSiSiS! l l i H H l H * * t * * * * * * t* * * * s t * * t * * 's * * * * r n t t t f M S f t M f i j iijiiitiiji S S S t S 3 iniCESsilg f //on** **1 P*** innTiw* :lOte <Ua*q Tm 14) Hat k n n I U w , k y X * * SSSSStiSiSSSSSSSSgSSSKSKSSSSSSSCCES . 'S p B l i S i !i 1 sssssss^ss iisiisiiii ?? ss S s iissss i i i i i i i s Hs s s H H I : 3~ I l i l l S E I ! I ! s assssrssss Sss S3S5S HsS=== 2 3S 3SSSS3 SKS5S3 s sss ssssss ssssss s ss =si _ni . s ........... i' 1 itili3 S B . . . ssksss: mmms s Ss k s Hs S ite ?6 sc ? 4 .ri- . SSiSSSSSSiSSSSSilSSCCSSSiSiiSSSSSiiSBSisSBSSSiiSSSSSSSCSS,, 1 IH M/it/ow*iM *** pu r w n w w k :ftiotO I p SI I 5S55K5K 5 i 5 i ii H H iiiiliiiiiis iiiiiiiiiiii iig i iiiii ii is ii. tss f asssssssbssbgsssssscssssassbbbbbikkkkbkksM hkEhiif ? m ? g g g g g iS S g g g m g ? m m g g g g S g ? ? g gSggggSgggg gggggJ gggg| w - s a a s 2 C 5 s c S s s s l - Ms c A i l - i i s s s i i i - ! : s s i . a s s B s i = =s . , s ; : ,, h ? ? Ta 1 4 : h t h u utf U w , h y 1 4 0 7 4 7 M : u n U u t ^ mn pnmt+d b y w h l O / Z t / l Q i n n U f y CJ.U>t*U-- et | Tw U S; S at t a iw U t, tk y I K t t* 2 0tay Q707M: lu U tttM l Mi f t U t a toy wahO/2/f xxxk x x x x . x xx P u w tlfy C lU r U Im part Tax IASs lU t Sax* a n t U w u , Day 1 * 4 Compound 3 name: suit (fiinc 3) Response Factor 179082 Response type: External Std, Area Curve type: RF 2 .3 2 c5 t Response- D*vay0707*: quanUtato4 *o4 prla** |py HltJMM iupoet H athod til: U s t nodiflad: Compound: fe in te d : Ci\HAmm\OovyO?079I.HtOM tthIVlfl2799b.udb Tbu O ct 2 0 1 :1 7 :1 2 1 9 1: W M (fu s e 11 Tbu O ct 20 12:ixO J 1099 Coapouad Di m : la u m l U f. : Quantify Trace; Cone, of Standards: User I I Value: Ui( feafc facto r: In te o rata tfindOM facto r: Chrouatooraa M il wledw: fOAA (fuite 1) t0M| TIC Cone. A 1.00000. Disabled 1.000000 2 .10 0 1.00000 Kataation TIm ( a l u ) : lU lativ a Aataatlon TIm : AT AaCareoea: TIm tflndoM (ainsi : faak Slection: 0.012. Raablad 0.000. Olsablad (IUM| 0.111 Oaacaat Aaspoese Typa: Aasponse: Batam a i Aroas folynoaial Typa: foint ( O iifis: f i t Weibtin?: Aaii Tcansfonutioa: XJLa*ar Include 1/X Nom Unita: faak-to-paak aapiltuda: 92 SaoothlnQ; tflndoM ira (scans): Nunber a i n o o t l f : Saoothino aathod: lo in v ailay tbrashold: ftaduca paak t a ill a * : fcalsa basaiina aaxiaua: oo Disablad 1 1 Savitsky Colay Orw v e r tic a l tbreshold: Oacace shoulders: Shoulder tAreekold: lU lativa baioht: Absolut hoiQht: lU lativ a acaa: Absolut* acaa: 2S.II Disabled S .00 l.SO, Disabled 0 . 0 0 . Disabled 2.00, tnablod 0.00. Olsablad 1 f E?E Ss;Si In : ?fr fs s S!S tt: 'if i liff i ?-i IS = |HS 8i ? ? 1 AM0 W o *> ft o o o gfgg m t *n VOM ft a * ^ ^9 1 s ^ e ft oe --O 1h f* $f m < ft mi :.^ i m i l pt? IS E2.SS 9 r;r r r? s s f f e?? *> ft II S i "" ? s s iil |s j .ss S < ; - t s?p if? it *fi* Ua ?f ES ? :i i I? s sr s l s p ? - ?S i? i * 2 ft ftM -- p* te r ! s: . --. . : i :5 !|jj M tO s S si " H i ir. j 1M=W ls e c ..ii 1 55 ; ii c js ** i il J i LI ? 1 Soo0B OSoo0 O*M03oe 12 SI u ae *! 5. 1sij as| 5 |jj5I biUl i l i ! X HM 3 m. 1 1 5 J.SS3 .... r i f i l i * w t* ssss si V1i =a jL 3 i -;*?*? l5 i s9 a i ** " 5m*mk* *J a: p issi P*''S-5'iS * 3 IP : 3 S Jf 15 3 -J li li r :.s 5 Si 111 U msJ i o o <So 4 O <n * 3 .. j ni 32! 5 -3 1 ! 3 ls III 33., 44 iSJSS H it ilsi DAVEY 070799: FACT Equipment Log 99077 Q uattro Ultima: 9261QB PAGE DATE: 10/27/99 ANALYST:mmh STUDY NUMBER: Tox 145: Matrix: Bat S3& UYgJ>ESCRJPTION; PQ A M ..93S FACT Method:ETS 8-51&8-7Q injection volume: 5 uL Cycle time: IO ir . Electrode: Z-Spm . Mobile Phase: <A12.0 mM NH4CH3CQ2 TN-A- or stndid number () 99085-11-3 (B)JsdeQH___ (B).m-a-294 5 _ Prepared (date/by): Expires: iAl 10/23/99 sah fAl 04/00_____________ m i 10/23/99 sah mi 04/00 Store at room temp? [v] or N Other__ Guard column: None________________ Part number: ua________ Lot number na Analytical column:J Size: 2 x 50 mm Part number 055-701-2 Type:_18__________ Sphere size: 5 um______ Lot number P9E11 Serial number 0591825Z Analytical param eters: Drying gas OThrl: 487 ESI nebulizing gas (L/hr)JO____ Sheath gas (L/hr)^. LC Flow rate: 300 uL/mia Bade pressure: 82 bar HPLC solvent gradient: 10min-10-95 Time (min,!____ 110.00_______ 21 1.00_______ 315.50________ 4 7,50________ 518.00________ 10.0 10.0 95 0 95.0 IM . Tuning Method Report Method: C:\MASSLXinC\DAVEX BACKUP JUJG99\DAVEX-RATS.PRO\ACQODB\PFOS-4 Printed: Wed Oct 27 14:31:21 1999 Page X 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 14B 249 Pressures Analyser Vacuum Gas Cell Rdbk OFF 4.3e- 3 Analyser LM Res 1 HM Res 1 XEnergy 1 Entrance Collision Exit LM Res 2 HM Res 2 XEnergy 2 Multiplier Gas Plows 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 Mathad: C:NMUin.YiaCNamO707ft.>IIO\ACQUM\llMEI('*<l*A*#M*ZS L u t M d ilia d : tad Oat 27 34:10:03 IMO cantad: t M O rni 77 1 4 :JJ:OS IStO M wt { nina ) : .O f u w t i w : 1 MN r 1 Ma* t a l r < Uf < } Catar Chana! Onlay 1[ Sacs ) r Span ( Dalton* 1 : S ta r t T1m ( Kin* 1 : Sad 71m I Kin* i : JUpaat* : OmiuwI f a r m O w fk u r 0.03 0.00 0.00 10.00 1 Dwell (Sac*) Cell Ksariy (#V) Cana ( V 1 <13.00 141.00 4.30 30 IS unction ; 3 MM IT 3 Mm a i r ( E li* ) I n ta r OmamI Delay 1 Saca ) : Span ( Dalton* ) : S ta r t Tina ( Kin* ) s Cad Tina t Hina ) : Mpaata : Chanaal faxaat Oauytocac 00..0030 0.00 10.00 1 D u ali (Sac*) Call Saatfy (aV) Cena I V 1 1 #10.0 70.00 0.30 0 0 tVroticn : 3 MM < 1 Mu* N U ( LIP- ) In ta r QummI Delay ( Sac* ) Span < Daltans t i S ta r t T1m ( Kins I : Cad Tina ( Mina ) : s Channel tarane Dawjhti <27.00 0.00 00..0430 0.40 1 0 .0 0 I CM11 (Sm s ) Call Ceaty I*! Can* ( V ) 0.34 40 40 i Method Report Method File: Lagt Modified: Printed: Page 1 C :\MASSLYNX\DAVEYO70799.PRO\ACQUDB\1Omin 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 Masslynx - Sample List Sample list: C:\MASSLYNX\Davey070799.PRO\SampleDB\102799b.SPL Printed Wed Oct 27 14:34:05 1999 File Name File Text 1 102799013 MeOH Blank 2 102799014 MeOH Blank 3 102799015 TQX145-RBS10229-H2O Blk-1, RWW 4 102799016 TOX145-RBS10229-Serum Blk-1, RWW 5 102799017 TOX145-RBS10229-1ppb-1. RWW 6 102799018 TOX145-RBS10229-5ppt>-1, RWW 7 102799019 TOX145-RBS10229-10ppb-1, RWW 8 102799020 TOX145-R8S10229-2Sppt>-1, RWW 9 102799021 TOX14S-R8S10229-50ppt>-1, RWW 10 102799022 TOX145-RBS10229-100ppb-1, RWW 11 102799023 TOX145-RBS10229-250ppb-1. RWW 12 102799024 TOX145-RBS10229-500ppb-1, RWW 13 102799025 TOX145-RBS10229-750ppb-1. RWW 14 102799026 TOX145-RBS10229-1000ppb-1. RWW 15 102799027 MeOH Blank 16 102799028 TOX145-RTS-9R03230M. Day1. control,-ext10/19/99 17 102799029 TOX145-RTS-9R03231M, Day1, control.-ext10/18/99 18 102799030 TOX14S-RTS-9R03232M. Day1. control.-axt10/19/99 19 102799031 TOX145-RTS-9R03233M. Oay1, control.-ext10/19/99 20 102799032 TOX145-RTS-9R03234M, Oayl. control,-extlO/19/99 21 102799033 TOX145-R8S10229-250ppb-1, RWW 77 107700033 MeTM-l ria n k 23 102799035 TOX145-RTS-9R03235M, Day4. control,-extlO/19/99 24 102799036 TOX145-RTS-9R03236M, 0ay4, control.-ext1C/19/99 25 102799037 TOX145-RTS-9R03237M, Day4, control,-ext10/19/99 26 102799038 TOX145-RTS-9R03238M, Day4, control,-ext10/19/99 27 102799039 TOX145-RTS-9R03239M. Day4. control.-extl0/19)99 28 102799040 TOX145-RBS10229-250ppb-1, RWW 29 102799041 MeOH Blank 30 102799042 TOX145-RTS-9R03245M. Day1, 5mg/kg, D50-ext10/19/99 31 102799043 TOX145-RTS-9R03248M, Day1, 5mg/ka D50-ext10/19/99 32 102799044 TOX145-RTS-9R03247M, Day1, 5mg/ko. D50-ext10/19/99 33 102799045 TOX145-RTS-9R03248M, Day1, 5mg/kg, D50-ext10/19/99 34 102799046 TOX145-RTS-9R03249M, Day1, 5mg/kg, D50-ext10/19/99 35 102799047 TOX145-RBS10229-250ppb-1, RWW 36 102799048 MeOH Blank 37 102799049 TOX145-RTS-9R03250M. Day4, 5mg/ko. ext10/19/99 38 102799050 TOX145-RTS-9R03251M, 0ay4, Smglkfl, ext10/19/99 39 102799051 TOX145-RTS-9RQ3252M. Day4, 5mo/ka ext10/19/99 40 102799052 TOX145-RTS-9R03254-1M, 0ay4, 5mg/ka ext 10/19/99 41 102799053 TOX145-RTS-9R03254-2M, Day4, 5ma/kg, ext 10/19/99 42 102799054 TOX145-RBS1Q229-250ppb-1, RWW 43 102799055 MeOH Blank 44 102799056 TOX145-RTL-9R03247-M, Day1. 5mg/kft ext 10/13/99 45 102799057 TOX145-RTL-9R032S3-M, Day4, 5mo/kQ. ext 10/13/99 46 102799058 TOX145-RBS10229-250ppb-1, RWW 47 102799059 MeOH Blank 48 102799060 TOX145-RBS10229-H2O Blk-1, RWW 49 102799061 TOX145-RBS10229-Serum Blk-1. RWW 50 102799062 TOX145-RBS10229-1ppt>-1, RWW 51 102799063 TOX145-RBS10229-5peb-1, RWW 52 102799064 TOX145-RBS10229-10ppb-1, RWW 53 102799065 TOX145-RBS10229-25ppb-1. RWW 54 102799066 TOX145-RBS10229-50ppb-1, RWW 55 102799067 TOX145-RBS10229-100ppb-1, RWW 56 102799068 TOX145-RBS10229-250cob-1. RWW 57 102799069 TOX145-RBS10229-500ppb-1, RWW 58 102799070 TOX145-RBS10229-750ppb-1. RWW Page 1 Page Position: (1.1) Masslynx - Sample List Sample List: C:\MASSLYNX\Davey070799.PRO\SampleDB\1Q2799b.SPL Printed: Wed Oct 27 1-1:34:05 1999 Page 2 Page Position: (2,1) MS File Inlet pile Bottle InjectVolume Sample Type Cone A 1 10MIN-POAA-980-IS 10mirv10-951 91 2 10MIN-POAA-9804S 10min-10-95f 91 3 10MIN-POAA-960-IS 10min-10-951 1 4 10M1N-POAA-980-I5 10min-10-95f 2 5 10MIN-POAA-96CHS 10min-10-95f 3 6 10MIN-POAAr9804S 10mitv10-95f 3 7 10MIN-POAA-S804S 10mm-10-W5f 4 8 10MIN-POAA-98CMS 10min-10-95f 5 9 10MIN-POAA-9804S 10mln-10-95i 6 10 10MIN-POAA-960-IS 10min-10-95f 7 11 10MIN-POAArB804S 10mitv10-85f 8 12 10MIN-POAA-980-IS 10mtn-10-95r 9 13 10MINPPOAA-98WS 10min-10-95f 10 14 10MIN-POAA-9804S 10rnin-10-95( 11 15 10MIN-POAA-9804S 10min-10-95f 92 16 10MIN-POAA-9804S 10min-10-95f 12 17 10MIN-POAA-98CHS 10min-10-95f 13 18 10MIN-POAA-98CHS 10mtrv10-95f 14 19 10MIN-POAA-980-iS 10nn-10-95f 15 20 10MIN-POAA-98MS 10min-10-951 16 21 1QMIN-POAA-9804S 10min-10-95t 8 22 10MIN-POAA-980-IS 10min-10-95f 92 23 10MIN-POAA-98O-IS 10min-10-95f 17 24 10MIN-POAA-9804S 10min-10-95f 18 25 10MIN-POAA-9804S 10min-10-95t 19 26 10MIN-POAA-980-fS 10min-10-95f 20 27 10MH4-POAA-9804S 10min-1D-95f 21 28 10MIN-POAA-980-IS 10mln-10-95f a 29 kJOMIN-POAA-980-tS 10min-10-95f 93 30 ' 10MIN-POAA-98O4S 10miiv10-95f 22 31 10MIN-POAA-9804S 10min-10-95i 23 32 10MIN-POAA-980-IS 10min-10-95f 24 33 10MIN-POAA-98O-IS 10mirv10-95f 25 34 10MHLPOAA-96WS 10min-10-85t 26 35 10MIN-POAA-9804S 10min-10-95f 8 36 10MIN-POAA-98Q-IS 10min-10-95f 93 37 10MIN-POAA-980-IS 10min-10-95C 27 38 10MIN-POAA-980-IS 10mirv-10-95f 28 39 10MIN-POAA-98O4S 10mirv10-95f 29 40 10MIN-POAA-980-IS 10min-10-95f 30 41 10MII9POAA-9804S 10min-10-95f 31 42 10MIN-POAA-98CHS 10mlrv-10-95f 8 43 10MIN-POAA-98WS 10min-10-95f 94 44 1QM1N-POAA-980-IS 10min-10-95i 41 45 1QMIM-POAA-9804S 10min-10-95f 42 48 10M1N-POAA-9804S 10min-10-951 8 47 10MIN-POAA-9804S 10min-10-95f 94 48 10MIN-POAA-98O-IS 10min-10-95i 1 49 10MIN-POAA-9804S 10min-10-95i 2 50 10MIN-POAA-9804S 10min-10-95f 3 51 10MIN-POAA-9804S 10min-10-95f 3 52 10MIN-POAA-960-IS 10min-10-95i 4 53 10MIN-POAA-9804S 10mi(v10-95t 5 54 10MIN-POAA-9804S 10min-10-95f 6 55 10MIN-POAA-980-IS 10mirv-10-95t 7 58 10MIN-POAA-9804S 10min-10-95l 8 57 10MIN-POAA-96CWS 10min-10-95f 9 58 10MIN-POAA-9804S 1Qmitv10-95f 10 10 -- 10 -- 10 -- 10 -- 2 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 QC 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 QC 10 -- 10 --* 10 -- 10 QC 10 -- 10 -- 10 -- 2 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard 10 Standard -- -- -- -- -- -- -- -- -- -- --* ---- -- -- -- -- -- ---- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- --- -- Masslynx - Sample Usi Sample list C:\MASSirNX\Davey070799.PRO\SampleDa\102799b.SPL Primed: Wed Oct 27 1*34:05 1939 File Name File Text 102799071 TOX145.RBS10223-1000pp6-1.RWW Page 4 Page Position: (1,2) Masslynx - Sample List Sample lis t C:\MASSLYNX\Davey070799.PRO\SannpleD8\102799b.SPL Printed: Wed Oct 27 14:34:05 1999 Page 5 Page Position: (2,2) MSFtte Inlet Pile Bottle Inject Volume Sample Type Cone A 59 10MN-P0AA-980-IS 10min-10-95f 11 10 Standard FACT: DATA REVIEW SUMMARY FORM Date: D ata Analyst: &s FACT Study*: 7 / NS T J&. .M atnx/T im epoinu: o a - D ata Review Sign-Off Aaafyit Rrrirw , . Kante/ Dale: "FA* ., , ,/ T e c h n ic a l R e v ira r (fase &*urAxA*/- fxt /3/t1fa tf thhN e m e / D u _________ Sample U ac Set-up A nalyst D aie/A naiyit: [rumimene S m j OJiA/fj Quality A m rance Review N am e/D ale.____________ Data Entry: M z u lesfo l Comment] / JuetM cadooi:___________________ A n a ta * : hAA (cut_______ AJAA ccestable L in e ar R a n e e LOO AM JAE x tra c tio n B la n k .................... RA2: Ha AMM a trix B la n k Calibration C h eck e AJA M S/M SD: G> AM U C II U s i l i thD ata S u m s ........... ________________ A n a ly te : (CH**) Ceptablc L in ear R a n g e -7..L M ffL l& ffL R"2: Q. 9 H 7 7 7 ________ M atrix Blank: A iS "fi-** & Calibration C h e c k * OK- .tUdf --7 'A' T ~K7` M S/M SD: K - ont, i / c - L . cAjA / A l l i t | r U ttD ata s u n n : d o s e d j c m j i |c t r \ 0 _ c L l A i 5 C L ______________" ^ j j l ^ c d llih J /tK , tlflK ------------ F u t yC r ? 0 M . J U t * U * J u .(------------ &r d rei. t n u J s t u j V e-vfU *. -fi** o J u . - J a s / s fa _____________________ S /1L/ u l e i d D a t'd 1 f.ftn O , kM s k J ~2* ttle r "M&*. 4 h - * ty t,c fi * . H id - . Jis iM s e jte lu /tc / 4rm. 'f it ._____ OtuVf. 4a tfisutfifj Jd<L ____ ~Hj J A*-a j Im k h a * . Q 4A.vftet.jd/* _____ i f i c c k J y<f h uakcfjan i t * J / w t b * 7 ~ /b - A & IJ c . - - 2k . l i g i o ih c f~ t f y h k J ie < n e c L t d /*> p y t'/c L 4- c jL v P rf- a ve* -iL n u t r '< &to*>rn<i. -h ^% E Jd*. A n a ly te PFoSa fO /l) Acceptable L in ear R a n g e */-Srk ~ LOQ: 7. JtSin-?gpKi________ li v n - J L 'H 3 L E xtracted B lank: fSS -/a*. OQ 4L LitiM a trix B la n k / c j i a CalibttooChecks: OK --0 A.4*_/*i>**i *"if-- - / r i MSMSD: lO au Sams: OK ____________ EnUmt -, IAV. 5 m u m \ d k M h n m - i l V k m v c -4 . __________________________ kjh rov-s-^ff FACT: DATA REVIEW SUMMARY FORM Dale: Otta Analyse 3 Dies Review Sign-Off A n aly st R*Ww ,, Nauta/Pate: T Z s 'V a ir /fl_________ FACT S tu d y * ------------ -------------------------- ------------------------------ T a c ta k a l * aiaw Malnx/Ttmcpointr U & ~ - . J A J - t t f W A ^ N - a / P u r ------------ U /i Set-upAnalyst Date/Atuiyjt: !tm u 1 -- ---- instrument Q 2m Analyte:, Siir r ----------------- NQu-n^/-DWate. .R___k _w__________________ Data Entry: (-AC- Cotnmtott/Jnstfikatios*: [Aoxptnhh C iac R u n e |LOQ :________ M ________ |RA* _______ HA----------CalibrationCheeltx -3L Ims/MSD:______ JA. [Data S tatu e F f--ITM PIm P MatrixBlank Z/4- lU S tru r i O <oO40Ooo*oMo*o w 4000 0O O O W M 440 u i i m m i i i m u i u h is u h j 40 440 0 -4 O 1-0 O O H U h O O O O 4l> O m t4H Q 4 440044440444 44n44l4n4n* 4S0O4O 4N4n4ft444440O4r4tn4M44n *O O I foO O O O r'4- SSSSISS 3| !I u. 2S3 m lili St t si =1 s * o* lili! flililil ><* ooooooS of 88fiS oSsVSa44rl0(Ss44*l0N*a4>44lVa4o4*4*co**4.* n2532ij3j2B35 so483i;84no4n*0| i ]iiii iii sa*i OOOOOOO* f'S i U!!l| os::ol!ns!ni!nilolOH54l0RiliSso IS!S0s0Iissl4|s j IIs s s s b sss 1 Iiiiillilllililisliiliiilililliilliiiiiiiiliiii 2 Z S S 2 * 8 2 2 8 8 8S 2222222222222222222 ft*00,0 0 5o<o .S :S S S !S S S 5 S S 5 S ?5 SS!:5 2 ;IS S S S S S S S S S S 5 S S S IIS S Issss5 ssssss2 ssssssssa ss sll2 2 3 ;ss5 ss sssssss J232S333233333333332333333333333333333332333323 i 1 I i 1 i I - j* i u * t : c t v i m a a o M n M .> > v M >i i w i\ m lu t h 1 (M i fri S H i M i l l 1 H attedi civ M w n a tM w ta iU K p tV M iu aitu u ii but tr i * as IM * J*M Cete: h -lM M li t r i ttr> a s I l l U t U l i a i 1 1104**001 3 1104**403 1 li04**aoi 4 1104**404 5 1104**00* 1104**444 T 1104**407 I 110***00* 9 1104**40* 10 1104**014 11 11049*011 U 1104**013 U 11049*411 14 1104*1014 15 1104*901* K 1104**014 1? 1104**017 1 1104*9014 1 1104**019 30 11449*030 21 110499031 33 1104**033 31 1104**031 34 1104**024 39 1104**42* 34 1104**434 31 1144**011 34 1104**01 2* 1104*103 *4 1104**410 11 1104**011 13 1144**013 I l 1104**011 14 1104**014 1* 1104**01* 14 1104**414 11 1144**417 I l 1104**410 19 3104**41 40 1104**040 41 1104**041 42 1104**442 41 1104**04) 44 1104**444 4* 119419041 4 11049*044 liitliV U t M R H*OM l l M t NtOK OUnk I M U l ' U S U U I ' B O * 1 1 - . H E t . 1 1 7 1 /9 * MC* raK l4 S -u sU flil-* r mec. 1 1 /1 / * MC* T O X l4 9 -B T S U 0 ) -ta r O U -9 . m t. U / ) / * MC* T O K lO - U S U m - lf * * - ! . 4 u rt. 1 1 /1 /* MO i a - i i i i u f - u i o i * ' i . u t , U / l / * * MOI T O ZliS-U SU O lf-aSfpO -. u t . X U M U u a iM M t P O O 'f , Mit. 1 1 /1 /9 * MC* l i / i / * * mm TTOo tEu Us -iu-wm umm<-tnoif4tir i.. mM . . U /)/* 1 3 /1 / Kl MC* T O U 4 S -U lU IJ M 4 tfo a -l. mm . 1 1 /3 /9 9 MC* iO H 4 1 - u iU f - T S a H * - i. mm . U / / MOi TOXl49-lB4ll039-100f0h 1. Ut . 1 1 / 1 / 9 * MC* *m IintiaMd aifrdt |M M >r4 lU M ld in a ili* taaUkurd TOU4S-*tSUai*-2S0pMr-lcrai4u. tU. *-1 11/31//91*/*MCM*C* T O X l49-T f-oaillO M -O -D a/ 2 1 . U t . 1 1 /1 /9 MC* T G X 1 4 S -m '* M J 2 4 1 K - -tejr 2 9 . a * * . 1 1 /2 / * MC* T O X U S -K T S -9 0 d m i* -* -A r 3 9 . a * t - 1 1 /1 /* * MC* T D X 143-U3U41*-294*pM -CCV9, u t . 1 1 /1 /9 9 MC* QC to u o -im > m )3 4 M M -o iir a, a u . n / i / >** TOXX41-NT*-9ft0324JM-0-Day 3 * . Mt. U / J / MC* TOX14i-RTS'9M 33S9M -Oaa/k0-Oty29. u t . 1 1 /1 /* IC* Y O X U S-*T S-9M 21SM -Sa/**-ew *3*. * . 1 1 /3 /9 MC* TOZ14S-tTS-*OOmT-Su/k>Oay2*- u t. U/3/** 4 T p x i i s - M i i o i y - H i a * c m * , t . u / i / mc* oc W l ) 4 S - m - U O U ) I M ' l M / l 4 ` O ty > l. u t . U / l / 9 MC* T O * :i4 5 -T S -**0ia9**-S u /lW -D ay2*. u t . 1 1 /3 /* * MC* TOU4S-MU3-23Q*pM-CCV. u t . 1 1 /1 /9 * ICS OC MaOll I l i a k 9O Z 14S-M U 11019-I30 B lk -9 . U t . 1 1 /3 / * MC* T O X I43-ftM U 039-*tra a lk - 9 . u t . U / l / 9 * NC* T O X U S -K T S U IJ I-tert l l k - 9 . a u . U / l / 9 * MC* t W 4 M U U I l - S o o l > . t . u t . U / * / * * MC* *c*nterd T O U l I - U S l i m - U U - t . U C . U / / * * MCa scaaterd T O X 1 4 S -a a sU 0 1 l-2 * M * -9 . U t . u / l / 9 MC* ra te a r W U 4 M U t f U M - M |* > . u t . U / l / 9 MC* ffia a d u tf TO 1 4 9 - U S U 4 1 * -lO O p v b -l. u t . U / l / 9 MC* fC M terf TO X 149-M M U 039-29|*M -9. U t . 1 1 /3 /9 * NCM ItU d ajrd I W I M U U m - i M n a - l . n e .1 1 /1 /* * MC* S t ter T O K U - 1 U U U M 4 4 * M 'I . 4 . U / l / 9 * mc* a c u te r T O X 14S-U lU 419-104*ul-. U t . U /l/9 * 104 | tu tee U au .J .n 2 4 .1 0 * .3 7 .0 * 2 4 1 .0 0 0 * 3 .0 0 7 1 5 .0 4 7 4 .0 4 2 4 0 .0 0 2 4 0 .4 0 3 4 4 .0 0 4 .9 3 1 .7 4 2 4 .* 0 4 .1 0 7 .4 0 2 4 1 .0 0 4 * 1 .0 7 3 1 .0 0 7 1 .0 0 El 7 .2 2 # 7 .2 3 0 7 .2 * 1 7 .1 0 1 7 .1 0 0 7 .2 4 2 7 .3 4 7 7 .3 * 7 7.24S 7 .2 1 0 7 .2 S 1 7 .2 9 1 7 .3 4 4 7 .2 S 2 7 .2 2 1 7 .2 S 3 7 .2 1 0 7 .2 2 3 7 .2 7 0 7 .2 4 1 7 .2 1 1 7 .3 4 4 7 .3 * 9 7 .2U 7 .3 1 1 7 .3 4 0 7 .3 7 * 7 .3 4 7 7.22S 7 .2 7 1 7 .3 4 4 7 .2 1 1 7 .2 2 4 7 .3 0 0 7 .2 4 4 7 .3 * 0 7 .3 X 4 7 .2 4 4 7 .2 4 7 7 .2 * 7 .2 3 4 7 .3 4 4 7 .2 7 1 1 .2 4 9 7 .2 1 0 7 .3 1 7 k m flu 13 MM i l mt 3 4 MM 2 0 M 7 2 U 0 MM s a c MM* 2 *2 MM S 37 MM a s m* 2 9 3 1 MM 4 1 4 4 Md 9 0 3 MM 13042 mt 172 4 0 MM* 1 *3 MM 39X4 bd 1 4 3 4 MM 1 7 MM 54 MK 5 1 MM 3 4 4 MM * 1 MM 39 MM 40 MM 92 4 4 3 MM 14 4 4 3 MM 4 1 7 2 1 Mb 4 1 1 1 MM 133 MM 147 0 0 MM 9* 0 4 1 MM 4041 bd 10 3 MM 7 Mb I l MM 1 *7 MM 103 MOC 3 24 Mb 1 9 4 MM 124 Mb 3 4 0 9 Mb 5714 bd 11072 M 140 1 3 MM 32*31 bd* O U . V tn e .o o o .o o 0 .0 0 0 .0 0 .0 0 . 4 . * 9 .0 2 3 0 .4 7 1 .2 0 0 .5 1 2 1 4 .4 4 4 3 3 .1 4 -1 -t -17 -13 -1 -23 -12 <70.42 - 124.53 -14 4 .U 3 0 4 .4 0 2 7 2 .1 4 0 .0 0 .0 0 0 .0 0 204.11 -17 * . 0 .0 0 0 .0 0 3 1 4 4 ,1 7 2 1 3 9 .1 4 1004.40 221.39 -12 1 .1 9 3TCJ.I9 4702.90 2 3 1 .1 7 3 .3 9 -7 0 .0 0 0 .0 0 0 .0 0 1 .4 1 1 0 .4 1 2 4 .7 4 -14 9 * 4 .4 4 114.27 2 7 1 .7 S 3 3 .4 1 1 1 .4 4 13 1 10 9 U 1114.1 U KW I34U I: (NMtlMt4 m 4 | t e ( 4 W l u U/I3/M I t tssK tsssasssE B SssssssssB sssssK B SC B cs 33 388 RR ita i l 3 R S te r c lIlllsIIS S lS lsiS H ls s II sllE sS g sg i ksb-shskkkSsIfcSbfcklkfesfcibssfehhfck? i--iS S i |S S5""33'fS',"-"|S^S',S"S"3'raST -TTgaTSariSTT-Ta z 335333:533533:52333333:333 5533:5333335:333 i i l l l l l l t f l l l l l l l l l l l l l l l l l l 1111I 111111111I 1 P girsl2Sll5lS5l5 H S5s333i53a3S33sS2sS55333I ssiS H ssisS S q J 355555555 5 5 5 533333533 9 ! i I 5 1 MAlHi MKlUttl U/AS/II QMMitr euitaMiw *>u w u it> rw Mn V at *m m i 1- rt. U/S/ff a ao itti QwMtltU* M l KlM*4 V 1m U / M / l l fOUU-ru Il/)/** H C l * i m i t i OUKlMt! by Im k i w u m * s s S i I 8* 3 l 1 \ *sji ntl li1 ! i i il t I* ! j3il2 1i **1 lit' sI un is J s *s| j s I Issi 2 lU S3 * S3 ils! 3?ll !j< SI JoLo vll*y U r n iwKic pik Mili 1 momo i. 1:1 li Il* JJ 3 I!IIi l i l i I a*jj S3 s 33W3 3U J |J | Si ss::5 ;t BUSH Hatkad sapere Mstbed ( lU i U i t M(UUa4: CMVMMd: Priacad: CiVNMStVa\asup414iy0.rVHcDOD\1144O.*db r r l Nrr 95 U i l t i U I* i l Murr (Chi) f r i im'* IS i t K i l l 1009 Csugtsund HaaMPt t a u m l ftaf. i Q u a d ly Traca: One. at lu a u c ttt Saar M Valu> Saar *ak Paccar: Xntagnraca Window Pactar: Oir--atogr-- Ma vladw i Surr IC*4 (Hens] rxc fix* 1.000040. Disabled 1.044040 2 .MO 2.40000 caseica Tina (nina) t elativa MCantlaa Tina; Tina Windau taina) > Saak la la c tie n : 7.311. tnaklad 4.444. Disabled 4.170 Honrase kaspons Tr** >ioMi h i l i w a i a l Typa: Point of Origini P it M ifhciag: Jud tr B ito n u c li i S ttsn al Arasa Um t neludo 1 OOM Onica: Mak-to-paak aaplituda: 11 Oaoocbing: Hinder at* (senna)i R a b i r 1 aanacka: nacotiitog Menadi tnablod 2 1 Join vallay tbrasbold: educa paak ta ilin g : alna k aaaiina wuanat: 10.44 344.40 5 .40 Drwr v a rtic a l tbrasbold: Dscsct shoulders: Showldsr tbraabold: 00.44 Diaablad 10.44 alati* bsigbC: Absolut height: a la ti aran: Absolues arasi 1.S4, Diaablad 1.44. Diaablad 3.44. Diaablad 4.04. Diaablad Quattro U, #6414E SOUP 020199: FACT Equipment Log 99092 PAGE W D A T E ;,U ^ M-22 ANALYSTaS STUDY NUMBER: TOX14S MATRIX: rat sera DESCRIPTION; day 29- dose & Control FACT Method: ETS-8-S-1 Injection volume: 10 uL Cycle time: 10 min. Electrodo* Z-Sprav Mobile Phase: /A2.0 mM KH4CH3C02 TN-A- or undid number (A ) 990?j - l b U _______ Prepared (date/by): (A)JSJQffi22jab______ (B).MgQH____ ( B ) TN-A-2997 (B) i m Q / 9 9 tali Expires: (A ) 04/00______________ (B).2010 Store at room temp? |Yj or N Other__ Guard column: None ____________ Part number na________ Lot numberja. Size:2 \ 0 mm_______________ Type:_CJi----------Part number. 0SS-701-2_________ Lot number: P9E11 Sphere size: 5 urn______ Serial numbcr:0591804Z Analytical parameters: Drying gas fLlhrl: 350 ESI nebulizing gas (L/hr) 13 LC How rate: 300 uL/min. Back pressure: 65 bar Sheath gas (L/hr)JL HPLC solvent gradient: lQmln-10*95 Time fmin.) i)jm ________ 2LLCQ_________ 3 ) JL 2 S _____ 4 ) 7.50 5ILQ________ J5EL. JM m o. 3 1 . 25JL 1QJL Tuning Method Report M e th o d : P rin te d : C i \K LS5LY N X \S0C T F02Q 199. P R O \ JL C Q D D S\PF0S3 KavT h u 04 1 4 :0 2 :2 7 1999 Pega 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 1.62 -41 -7 150 250 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier Pressures Analyser Vacuum Gas Cell Rdbk 5.1e-5 4.Oe-3 MS2 LM Resolution KM Resolution Collision Ion Energy Ion Energy Ramp Lens 8 Lens 9 Multiplier Sat Rdbk 14.0 14.0 0.9 Q.O 4 650 3 Set Rdbk 14.0 14.0 10 2.0 0.0 40 0 650 7 36 1 i 's j J iS 2. n fs i ! I 1* i !ij! |3 1 !I 2 lili! I i i i 3 I iU i 3 .- S is 1 1 ;1 ! liil 3SS" jij ! ! Alil;l > I >- H r w c C M u gktw Dm U <Sca) C U C aargy (VI */* '{ . iI Mat b o d l u p o r t U m t'b o a Til Uac MediCl#41 Printedt c iucMn.noc\<ovtoaoift.tnovAcoaoBUfiMixi-xo-93 nuradty, Korabr 04 if* Ilt22i29 Thursday, tforeetoer 04 1939 13iil:3l Fmg 1 D1100 tC fv p Xaltial Conditions Solvents A% B% Cl D% 90.0 10.0 0.0 0.0 Flow (ral/min) Stop Tine (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 1100 LC Puep Gradient Timetable The gradient Tinetable contains 5 entries which are : Tine M 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 9S.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 Pressure 400 400 400 400 400 100 LC Pus External Brest Timetable t 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 Contactl Off Off Off Contact* Off On Off 1100 Autoe*nc>lr initial Conditions Draw Speed Eject Speed (til/min) Draw Position (mm) Stop Tine (mins) Injection Volume(ul) Vial Number 200.0 200 0.00 9.00 10.0 51 Maaalynx - Sample List Sample List: C:'MASSLYNX\soup020199.pro\SampleOBM10499a.SPL Printed: Thu Nov 04 13:18.22 1999 Pag 1 Pago Position: (1 , i) Fila Name Fila Text US Fila 1 110499001 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 2 110499002 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 3 1 1 naaanna nisnk 10MIN-PFOS-POAA-PFOSA-IS 4 110499004 TOX145-RBS11039-H2O Blk-9, axt. 11/3/99 MCH 1OMIN-PFOS-POAA-PFOSA-IS 65 110499005 TOX145-R8S11039-Sera Bik-9. Xt 11/3/99 MCH 110499006 T0X145-RTS11Q39-Sra Blk-9, ext. 11/3/99 MCH 1QMIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-1S 7 110499007 TOX14S-RBS11039-5ppt>-9, exL 11/3/99 MCH lOMIN-PFOS-POAA-PFOSA-IS 110499008 TOX145-RBS11039-10ppb-9, axt 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 9 110499009 TOX145-RBS11Q39-25ppt>-9. axt 11/3/99 MCH lOMIN-PFOS-POAA-PFOSA-IS 10 110499010 TOX145-RBS11Q39-50p0t>-9, exL 11/3/99 MCH lOMIN-PFOS-POAA-PFOSA-IS 11 110499011 TOX145-RBS11039-100ppb-9, axt 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 12 110499012 TOX145-RBS11039-250ppb-9, axL 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 13 110499013 TOX145-RBS11039-500ppb-9, axL 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 14 110499014 TOX145-RBS11039-750ppb-9, exL 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 15 110499015 TOX145-RBS11039-1000ppb-9, axt 11/3/99 MCH lOMIN-PFOS-POAA-PFOSA-IS IS 110499016 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 17 110499017 TOX145-RTS11039-250ppb-MS9, axt. 11/3/99 MCH lOMIN-PFOS-POAA-PFOSA-IS 18 110499018 TOX145-RTS11039-2S0ppt>-MSD10,xt 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 19 110499019 TOX145-RTS-9R03240M-0-Oay29, axL 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 20 110499020 TOX145-RTS-9R03241M-O-Day29, axt 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 21 110499021 TOX145-RTS-9R03242M-O-Day29, ext 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 22 110499022 TOX145-RBS11Q39-250ppt>-CCV9, ext 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 23 11 0499023 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 24 110499024 TOX145-RTS-9R03243M-0-Day29, ext 11/3/99 MCH lOMIN-PFOS-POAA-PFOSA-IS 25 110499025 TOX145-RTS-9R03243M-0-Oay29, ext 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 26 110499026 TOX145-RTS-9R03255M-5mg/kg-Oay29, axt 11/3/99 MCH lOMIN-PFOS-POAA-PFOSA-IS 27 110499027 TOX14S-RTS-9R03256M-5mg/kg-Oay29, ext. 11/3/99 MCH lOMIN-PFOS-POAA-PFOSA-IS 28 110499028 TOX145-RTS-9R03257M-5mg/kg-Day29, ext 11/3/99 MCH lOMIN-PFOS-POAA-PFOSA-IS 29 110499029 TOX14S-RBS1103S250ppb-CCV10, axt 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 30 110499030 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 31 110499031 TOX145-RTS-9H03258M-5mg4tg-Dav29, axt. 11/3/99 MCH lOMIN-PFOS-POAA-PFOSA-IS 32 110499032 TOX145-RTS-9R03259M-5mffVfl-Dav29. axt 11/3/99 MCH lOMIN-PFOS-POAA-PFOSA-IS 33 110499033 TOX145-RBS11039-250ppb-CCV9, ext 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 34 110499034 U iiO H RUnfa 10MIN-PFOS-POAA-PFOSA-IS 35 110499035 TOX145-RBS11039-H2O Bik-9, ext 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 36 110499036 TOX14S-RBS11039-Sera Blk-9, axt. 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 37 110499037 TOX145-RTS11039-Sera Blk-9, axt. 11/3/99 MCH lOMIN-PFOS-POAA-PFOSA-IS 38 110499038 TOX145-RBS11039-5ppb-9, ext. 11/3/99 MCH 10MIN-PFOSPOAA-PFOSA-IS 39 110499039 T0X145-RBS11039-10ppb-9, ext. 11/3/99 MCH 10MIN-PFOSPOAA-PFOSA-IS 40 110499040 TOX145-RBS11039-25ppb-9, ext. 11/3/99 MCH 10MIN-PFOSPOAA-PFOSA-IS 41 110499041 TOX145-RBS11039-50ppt>-9, axt. 11/3/99 MCH lOMIN-PFOS-POAA-PFOSA-IS 42 110499042 TOX145-RBS11039-100ppb-9. ext. 11/3/99 MCH lOMIN-PFOS-POAA-PFOSA-IS 43 110499043 TOX145-RBS11039-250ppb-9, exl. 11/3/99 MCH 10M1N-PFOS-POAA-PFOSA-IS 44 110499044 TOX145-RBS11039-500ppb-9, ext. 11/3W99MCH 10MIN-PFOSPOAA-PFOSA-IS 45 110499045 TOX145-RBS11039-750ppb-9, ext 11/3/99 MCH 10MIN-PFOSPOAA-PFOSA-IS 46 110499046 TOX145-R8S11039-1000PP6-8, ext. 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS Masslynx - Sample list Sample Ust C:\MASSLYNX\soup020199.pra\SampleDB\110499a.SPl_ Printed: Thu Nov04 13:1822 1999 Inlet File Bottle Infect Volume Samp* Typ Cone A Cone B Cone C 1 10min-10-95 91 2 10min-10-95 91 3 10min-10-B5 91 4 10min-10-9S 1 5 10min-10-95 2 6 IOmin-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 10mirv-10-95 9 13 10mln-1O-95 10 14 IOmin-10-95 11 15 10min-1O-95 12 16 10mir>-10-95 92 17 10min-10-95 13 18 10mir>-10-95 14 19 10min-10-95 15 20 10min-1O-95 16 21 10m>n-10-95 17 22 IOmin-10-95 25 23 10min-10-95 92 24 10min-10-95 18 25 IQriiin-tO-95 19 26 10min-1O-95 20 27 IOmin-10-95 21 28 10min-10-95 22 29 10min-10-95 26 30 10min-10-95 93 31 10mv10-95 23 32 IOmin-10-95 24 33 10mirv-10-95 25 34 10min-10-95 93 35 IOmin-10-95 1 36 IOmin-10-95 2 37 IOmin-10-95 3 38 10min-10-95 4 39 IOmin-10-95 5 40 IOmin-10-95 6 41 IOmin-10-95 7 42 10mi(v-10-95 8 43 10min-10-95 9 44 IOmin-10-95 10 45 10min-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 -- to -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- ------ ---- ---- -- ---- -- -- -- -- ------ -- -- -- -- -- ---- -- ---- -- ---- -- ---- -- -- -- ---- ------ -- -- --' ---- -- ---- -- -- -- ---- -- -- --* ---- -- ---- -- ---- -- -- -- --* ---- -- ---- -- ---- -- ------ ---- -- ---- -- ---- ---- -- ---- -- ---- -- ---- -- -- ---- ---- -- ---- -- --* -- -- ---- -- -- -- -- ---- -- -- ---- ---- -- ---- -- Page 2 Page Position: (2.1) FACT: DATA REVIEW SUMMARY FORM Date "In f a D a n Anaiyjt: FACT Study #: 15* N s M alnx/Tim epointa: r Sample li e /toSffU ftijr jj/*c - ____________________________ _ _ _ _ _ Set-up Analyst D ttc/AnalyiC MMH dfos-hl liutrum cnC & Z tL A flih tc : P#A ca/r) MA ccentable l i n e a r R a n e e a LOO: fA RA2: ma C aitbm ioa C hador HA M S/M SD: iJtfi D ata S tatu s VfiTfru-ffl MAE x tra c tio n B lank: MAM a tr ix B lank: A n aly te: I& IJSm -_________ Acceptable L inear R a n g e . 'J&ppL LOQ: J ^ L E x tracted B lin k : jess -Ama. X R-2: o. n is r to M a trix B lank: < 8 -f**- >Q Calibration C h e c k s OK ~~ ( ~ i`A ) MS/MSD: Kilfc-________ _____ Data S tatur Did Review S ip -O D Aflatytt RrrW w N am e / D ate. J * c */*/** T echnical R avlaw N a m e /D a te : Jfrt? . ._ j Itjh h W -V 'ff Q uality A aaunanca Review N a m e / D a t e : ________________ Data Entry: _ * L J \ C om m enti/Jita tiik a tio a i: Q A (JiitrtJlK - /V t/W MstS A c / Ymk- y H * A . j h X . j* iL S tfa f y re*. <*</ f a c / , x -j-ttMiS d t, . '* * * __________ 1-BkJ f'jiLtttWvt- >*ia f . f j p l a ^ / 9 ^ ij> L .I X U C ic lluu t Jie Attir JAt a6.~ 'f a y fa r e J u . t i m a -,,. T fa *& >'/> C C& m j '^U fyrK t.td s. J - fa M t a J lL k -A t SKt-iVS fiK rrt___ flkJu Jfa OOLUKtrriLAfm /-y / a n f e f f rw ''afa I 4 ` - zJ * s "fahl_______ ^ 'X tJ itm J s i j Are*. CiKn,/t o>*- __ S f-r -s b i___j& __ A m a if a . __~fa-- - Jt& rfta*. fa lc A r J A S "Al[<r<i A n a ly te TFoSA ((Hi) Acceptable Linear R a n g e f- f jp L $T ?. LO Q :. M p k . *"* o - m m E x tracted Blank: ItSs f L t 0Q -CtLM a trix B lank: /< X r tfc x . Calibration C h e e k r OK = __________________________ M SM SD: D au Sacue illA - di FACT: DATA REVIEW SUMMARY FORM Dale: D u Analyse t/f t ___________________________________ _ _ _ _ _ 7AS :FA CT S tudy _fof NS_____________________________________ _______ M atna/T ienepoiou: & / - th j & df< j 6> *kl Sample Lin: t gSiti ffcfa Set-up Analysis Date/A nalyst .. M*\!f ,/*>m ____________________________ In stru m en t: b y , a w f f ________________ ;_____________________ Data Review Sign-OIT A nalyst Review N am e/D ate 3 S tf /t T echnical Review A f ij k rN a m e /D a te :-------- t pO jjA - O h /. Q u ality A jau ran ca R eview N a m e / D a t e : _________________ kD a t a l a t r y : ______t t.t.C b r jity^ On. li U C O/Vf/ LAC Ii A/?? S in {l/A ? ^A nahit: __________________________ _ AJAA cceptable L in e a r R a n g e ; LOO: aJa A/JtE x tin c tio n S ln n lc _____________ R -2 : A n_______________ Calibration Cbeeksc _______ AfA MS/MSD:_____________ ~~----- M a tr ix B la n k : /W * __________ D ata S t a t u e _______________________ SSSSSSSSKHBKSSSSGafiEES lili! i'S'sPf* h " im h s% Mf r ii* ?? n mb I I" ! n il i fili : :a:j 3 Si ! l! i =:i. I l i iiiliil bkbbkik i S'aSSsSSSSSSS SS5332 5 5 SH 55555S5 =s 33sts; SEBEES 55SS5ES3SS| m i m i m i vinti m i n i m u m : bssssssasss abissi: ssssiB ssisssbssf Es.ssv.3 b a is s s ...ssk i i i f ! I t I i i : llKlb I tllIliS S is a s Ilillis liis ll S s s S ? 3 e 5 S e K e . . . . S S E 3 S r S s g s e s B>Ms saasstasesssssjisssssssssssis _..iS 3 -V.-5C i I zzi** xkisse 1 m im m ,\ m m m m i m i r u f i ^ i r m u s rrr?rr??r? SSSSCSSSSSSS s b c c c s r s s s s s s t s . . : . . u ^ -s s s j. E .,..,.,.5 f i i ___________________________:-----------------------------*** a(*hi f . L H O wwtlfr C itita r u ia a Mi n t CU(l*4iylt Miai mm 4b m - m . u /)/H f **09 X rlUMl k r U i U/M/M U IM iC r Ca IUMi U M M it n u 4 i 4 * r i o m n i ad M- t u t . n / t t * * N 2 Q201Ml OMtltMM ICiK4 toy ito* U /M / VUMlCy CsUte(ton lip iift KU41-*r2i contrai 1*4 oM- m . 11/3/** 3 M * MMMI uM tlutpd and prime* by 1m m U // * Matter e U k m (M Mart T C U tl'ttyU Mktral am * om- m i . U O / t l ( 4 U /M /St tili rsjg r ss : W 9 mm [U* Ifll U n Hg' *. ^ vnK>*1SfcS |:|?*ss s ?i i<.. 15 rt ? ft. ft. - B *pr. t s* ri * S *'2 c ; S M t t M d Ki. Oft HthOd :.* U aat u o d ilia d t C om pound: 9T&AIM1: Ci\H.MSl'ttnva2i:p':9199.ro\Natii0SUlSb.a4b K an .'V C J : : : U 1 * 9 2 : t :s ice: H o n :::: v 0 1 2 7 : 2 5 : 5 4 1 9 * 9 Compound MUM: I trival K (.i Q u an tify T race: C one. o f S tandard;*: B aar * f V alue: O u r te a fa c to r: X n te?r t iin d o v re c to r C h re M C o c .'* * * a a e w ind-. S e c a n t i e r T;?m i in ? : b e l a t i v -it a c t i o n Tip:* * T M l a r t -C<: T tia e W indow < n i n a l : taaV S e le c tio n : res e tu i U -'cr.a J T IC Cone. A 1 .0 2 7 1 9 9 . D is a b le d i.cc:: :.c :;:a a T.:i:. e n a b le d D isa b led 2 .122 b aap en ae T ip * : M a p o n ia: P olynoaual Typei S e in e o f O rig in : F ie W o L fM :r.j: JU ia T r*. j::r% a tis r : L if.ee.S xeZ vfe .Ten O n ita : F o a k -to -r . : apl itc -ia : S m co th in ?; V in d o v a i : (a c a n a ): M u o u r o f aw oot& s: ta s r c h in g :h o d : Sr.v il ad l J o in v a lle y chr*hoId: O advci p*< S a ia a b a .-iii:.* oaaiauait D rav vr* th r * .'.:2 d O atacc a .d ri: S h o u ld r :: r e a h o l d : 1 0 .0 0 5 .:: ; d 12.c: b e la tiv * A b so lu te A alaciv e A b so lu te i .. a : >r<*: 2 .2 2 . 5 .;:, 2 .9 2 . O iaab lad O iaab lad O iaab lad o ia ab la d 0 2 ecsr ODDO liti luthoil dipoi M othod ( U c U n B odlilO d Caapouad: P rinted; C:U SU A m s-:- .':Q lt ^ to V M tW M 'a ie S 9 t* -* d b Hon ;;OV 0 T ;;.- ;S S 1999 s - r r (CM: Moa M w ft 0 7 .C -.S * 1999 C cp o im d ::m n : la ttriu l xf. ; Q uantity T u e : Cone, of ic tn d ird i: U * r RF V*l u : flo o r Rook r * c o r : I n te g r a te W jnJov F a c to r Q u o M tO ';:* .'* au * w u v to -: S- TZ (C hi) (::sr.*) :.c :? a o o . ci*biod :.c :;io o .s : : , : . :;s* R e t e n t i o n Tica* l o i n ) ; R e la tiv e ;encvon Tin RT Tiaac W inde* ( m i n i h Peek S electio n ; e n a b le d . O iaeblod 1 o.: t aeareat R*a?Ona* T ype; Reapona*; lolyaeai) Typ; P oint of 0 r7 n : P ie W oigf-.tir.;: R u la Tr*.-.i:`3 5 \ tio n : rr.tT n a l ia ti L tsaar tx zl-ji l/x . Ses* U nit*. Peakto-p*k ap U tu d e; S *oat!\:r.: Window a i t c a c o n a ): Muaber o l la o o tM ; Ruootfcing rtt.-.o d : Z ra lltd Jo in v a li;-- th resh o ld : Reduce p* . t a i l i n g : R o is ba <'.i~a M xianun: Draw v e r t i r tM o c n o ii: D etect a .-;:;j* ra : Shoulder th re sh o ld : R e l a t i v e ` e ig .'m R batluee ..e ig h t: R elativ e ara! A b etin e arto : 93 .:; ;iA ii* d 33.c ; : . * .. oiM hl*d Z . . . D iabl*d z .c ;. oioahlad 3. : . D U eblod Pa Quattro IM 6414E SOUP 020199: FACT Equipment Log 99092 PAGE 1/1 DATE: 11-05-99 ANALYST:mmh STUDY NUMBER: TOX145 MATRIX: BUjga_PESCRIPHONL<ky.2&dil FACT Method: ETS-8-S.I Injection volume: lOuL Cycle time: 10 min. Electrode: Z-Sprav Mobile Phase: (BlMcOH TN-A- or stndrd number (A) 99085-11-15------- (B )JfM :2327_ Prepared (date/by): Expires: (Al 10Q0I99 h --------(AjJM ffl------------------------ (B) 2010 Store at room temp? @ or N Other:. Guard column: None________________ Part number: na________ Lot number: pa Analytical column:.Kcy39nLBSail__ ____________________________ Size: 2 x 50 nun ___________ Type:_ll__________ Sphere size:_3_urn______ Part number. 055-701-2_________ Lot number: P9E11 Serial number:05918042 Analytical param eters: Drying gas (L/hrl: 350 ESI nebulizing gas (L/hr) 13 LC How tale: 300 uL/mitv. Back pressure: 65 bar Sheath gas (L/hr)Ji___ HPLC solvent gradient: lOmin-10-95 Time (min.l D OPO 2 1 1.00 31 5 .5 0 4 1 1-50 5UL__________ _%B JM l& JL JS. 25JL 10JL T u n in g M ethod R e p o rt Method: C :\MASSLYNX\SOUP020199 ,PR0\ACQUDB\PP0S3 Printed: Pri Nov OS 15:32:05 1999 Pepe 1 MS SOURCE ( ESP- ) Capillary Cone Extractor y-< RF Lens Source Block Temp. Desolvation Temp. HS2 Sat Rdbk 1.60 40 50.2 150 250 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 Len3 9 Multiplier Sat 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 uwiiu MtM KM : Ct\KuaLTKX\eoGB-03ai.r*oiAogosoU< b u t NMU(t4: fr i o n is if rru u d ; r r i aw u ifiliil x**9 nM-MU-nuA-z M tt M ay ( BUM ) < a.a* iMOCtlM t 1 MMMOf 1 Moo f a i r 1 MV* ) l o u t CMMwmI Dalay ( Saco ) i Spaa t Dal com ) : S ta rt Tino ( Kina ) tod Tina ( Kino } Speata ( Clunaal tarase niuQhtar 0.) 0.00 o.ao i.a i Ml Itaca) C all Worai <av> COM ( V } 1 13.00 14.0 . 3ft 30 19 flMCtlOB 1 3 MUI of 1 Mao P a ir ( OF* I Xntar Choanal Dalay i1 Soca ) * pan ( Daltoao } < S ta r t Tioo ( Kino ) i Dad Tino 1 Kino t apaata : Choanal taran t Oauphtar S.03 . la.a i Duali (MCI) Coll snorry (on Cono ( V i ta .at .DO .l 49 4 Function i 3 MW f 1 Mom to u r ( MW- ) lo car Channel Data/ I: Saco 1 i Span ( Oaltoaa 1 j S ta r t Tina ( Mina 1 t Mad Tina ( Kina ) i feepaaca : Chincoi tarane Oauphtar 0.03 8.00 a . oo la .o o i Duali (Saca) Coll Maorpy lav) Com < V 1 4.00 70.00 0.30 49 40 Naetlea t 4 MM of i H ui f a ir 4 n r * ) Xator Choanal Dalay ( Saca i t .*3 ( D iltS M ) I t.M s t a r t Tina { Nina ) : o.oo KtoadpTatitniai ( Mina I : 118.0 Channal ru M t Daughter Sn U (Soca) Coll Oaargy <aV> Com ( V) 1 427.80 00.00 .J0 40 40 ** X Masslynx - Sample Ust Sample Ust: C:\MASSLYNXNsoupO20t99.proVSampleOB1110599b.SPL Printed: Fri Nov05 15:26201999 Page 1 Page Position; (1 , 1) File Name File Text MS File Inlet File 1 110599028 MeOHBlank 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 2 110599029 MeOHBlank 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 3 110599030 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 10mln-1O-95 4 110599031 TOX145-RBS11039-H2O Blk-9, ext. 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 5 110599032 TOX145-RBS11039-Sera Blk-9, exL 11/38 MCH 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 6 110599033 TOX145-RTS11039-Sera Blk-9, exl. 11/3899 MCH 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 7 110599034 TOX1 45-RBS11039-5ppt>-9, ext 11/3899 MCH 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 8 110599035 TOX145-RBS11039-10ppb-9. ext 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 9 110599036 TOX14S-RBS11039-25ppb-9, ext 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS IOmkvlO-95 10 110599037 TOX145-RBS11039-50p0b-9, ext 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 11 110599038 TOX145-RBS11039-100ppt>-9, ext 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-1S 10mln-10-95 12 110599039 TOX14S-RBS11039-250ppb-9, ext 11/3899MCH 10MIN-PFOS-POAA-PFOSA-IS 10min-10-9S 13 110599040 TOX145-RBS11039-500pp6-9, ext 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10mn-10-95 14 110599041 TOX145-RBS11O39-750ppt>9, ext 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 15 110599042 TOX145-RBS11039-1QOOppb-9, ext 11/3/99 MCH 10M1N-PFOS-POAA-PFQSA-IS 10min-10-95 16 110599043 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 17 110599044 TOX145-RTS-9R03255M-5mo/kg-Oay29,0:10 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 18 110599045 TOX145-RTS-9R03256M-5mg/ko-Day29, D:10 10MIN-PFOS-POAA-PFOSA-IS 10mln-10-95 19 110599046 TOX145-RTS-9R03257M-5mg/ko-Oay29, D:10 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 20 110599047 TOX145-RTS-9R03258M-5mgrt<B-Day29, D:10 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 21 110599048 TOX145-RTS-9R03259M-5mort(0-Day291D:10 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 22 110599049 TOX145-RBS11039-250ppb-CCV9, ext 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 23 110599050 MeOHBlank 10MIH-PFOS-POAA-PFOSA-IS 10min-10-95 24 110599051 TOX145-RBS11039-H2O Blk-9. ext. 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10mln-10-95 25 110599052 TOX145-RBS11039-Sera Blk-9, ext 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 26 110599053 TOX145-RTS11039-Sera Blk-9, exl. 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 27 110599054 TOXI45-RBS11039-5ppb-9. exl. 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 28 110599055 TOX145-RBS11039-10ppt>-9, ext 11/3/99 MCH 10M1N-PFOS-POAA-PFOSA-IS 10min-10-95 29 110599056 TOX145-RBS11039-25ppb-9, ext 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 30 110599057 TOX145-RBS11039-50ppt>-9, ext. 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 31 110599058 TOX145-RBS11039-100ppb-9, ext 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS IOmin-IO-95 32 110599059 TOX145-RBS11039-250ppb-9, ext 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 33 110599060 TOX145-RBS11039-500ppb-9, ext. 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10min-10-95 34 110599061 TOX145-RBS11039-750ppb-9, ext 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10mln-10-95 35 110599062 TOX145-RBS11039-1000ppt>-9, ext 11/3/99 MCH 10MIN-PFOS-POAA-PFOSA-IS 10mlrt-10-95 FACT: DATA REVIEW SUMMARY FORM Dale j 'M l . fri D ata Review Sign-Off A nalyst Review Nam e / Date: , I S !l y _________ FACT Study: M atrix/Tim epoints: ~T)n* 1* / Sample Lilt: /o/iffo. Aidra! e Ai-t . cd. Ad f f ' 7' Set-up Analysis D ite/A m Jyst: >`hs In 7*s T ech leal x rN am e w /h* Iii/n Q u ality A ssu ran ce Review N a m e /D a t e : _______________ D ata E otiy: w IM o h i/v In strum ent: Sj Lp s z Hf i ____________________ A nalyte: TaAA^Of l ' ) ^ ___________________ Acceptable U n e a r R anae: / / > C e ru d SJHuldL S e e fyiuMtuJs LOO: AM E xtraction Blank: R*2: ^AM a trix B lank: Calibration C hecks: HA M S/M SD &tr- & U l l o l A w ________________ D ata Status: rr JS> A n a ly te : __ - 2 ^ L j S i Z L -- -- )efo/rf 2 M &-70A cceptable L in ear R an g e: --------- Z ____________ LOQ: _______ -U . LagE x tracted B lank: /d > e m R-2: O . m W M atrix B lank: (etc - a . . Lod OKC alibration C h e c k s: -- /i "/ ^ Com m ents / Ju stifk itio iu : as aa/ fy*-r*st*J- rn cd iLh-tdi" - __ * . . & / [ ! ------- .cLteJcs ^ ir e e - f n t i c / t X ra - " / c ______ U iu A d Jd *- -fty &AA__________ t -3L~j>Lt eLauJJ he reriLt r*>M e h L . -- / % toltoli*_________________ ^ 7/. .v</ t t l + j j j , tu*.** Jx. d ,S ta i.J - L fT C insi ~ iitj d ji[ ta d : dLt /naa.K - A C W t*-__ T jU jttS * Pol' S.)as dryjL jJ S j -H~*d___ '4Lr /fea ti-~J tk+lin. L f - S o s y%.~ 4Lc Lag,. S m * , s t - y L * MS/MSD: OK______________________________^ I K . ^ k u d 'dtf<i'/t`%`S 0**- <rf X id xs!. Da Status: & l W VtoDliuWxt J O d U _____ !__ JM t- Y C J/jj- b i b - L td A n aly te: TF*SA CCHZ), M h d l ^ t b L J s / - $ < * b i f f i s i ____ h .>j j lA cceptable U n e a r R ange: i!i ^ ay* L 0 Q : _ j 2 J ^ c ____ E xtracted Blank: (rtf -/i*-*-log R-2: . f n S f f M atrix BUnk: /~ c c ? Calibration C hecks: -- & y - /w w -- ~ 3 ^ / * C~W"/) M S/MSD: JDfc. . L iv i ,a> *. A a ry te tt'.__ ~ -fai ___ 7t-c 1ZJ fffr ., #d, l $ Mf - l t r i + r, 'fad-Is.__ UWUfL- uea.au. 'U t y d 'J d f fd~. JKlLjAll* : l*I***-- *<-. & U.VUX. c)o Li. lUjtci Data Situa: E f t W l 1________ J O ^ h l M i* *<**"')#o**t Llmilt IM Ze-/uj-ri s o u r c e , ia t o / S f f ^ j C .A S r y - W f lA A iS tw o T )* IU ( i f FACT: DATA REVIEWSUMMARY FORM Dale: i*itih i D ala Analyst: FACT Study*: M atnx/Tim cpotnu: Samp} Lut: // T t j if /O K rti Set-up Analysis D ate/AnalyiL . f/ V /W y H S J i /ht Data Review Sign-OfT A nalyst Review N am e / Date: 3 -S / - / / f / f y __________ rfultf Technical Review n , Name t Date:_____ A ller 4~o Q uality A sso n ile Review N a m e / D a te :______________ _ T -o ____l . p t X U - lo b iv , D a t a E n tr y : __ I k L __ ioIu h * C o m in e a ts / J u t d f k a t i o m : ___________________________ _tfy*KS . Dx-c r/ */C CoaX/ Stey^e jjg L e i f A # - .,S ik tJ ^ i s J k S L A re lift, ft s * b/A S H a b e r * Jif' * u * h -Q d ^ s H&Hs/r&f o f ~h - Ita le. M s h J d s te U e r tiL ~~3*$ t f / t / t l 0 Ar**. C d l / r r if c 7STi> |KVt 0 ^ ^ S z + jb * k * J Jti/ia .y ro u t/j-T .^ .A?./T u c r tr f__ -ZffleLi__ ^Buii*a~yo r J --ilOJJA*.__&._______ A fijA iw * .___ H _ 2 $ s /S 1 jfVK- /rJ P fd -^A /rg-o--v- gfratA w . H /Lm-ret Pv=a A/rrf /v& rh -rS e f r --ite * *=/<u I rsBsssssssrsssssssiitsssssssKssssssssssssssBssssssssBss....,....*.* ss ss 88 8 8 S ss Ss s s P ::s i l SSSSSSSKC ih h ih 5 S S S E SSSSS S SESEES 3EES2S S.EESEEESSSSESEGS i u m i m m sm m m m m m m m m m HHe e. 5 .5S3 . 5SSS S Ssee s.. IS3 S.S.i. S.SSSs3g. .s 2S3SSSES8 8 SS tS S S K S S S 5 3 S 8 S 3 3 S g c 'S SSSiSCSSSsb'sSSb *S555 8 I s ss & eS| 5 ? ! ? ? i ** >! ta a il lM u 4 >UkI tar 1m ! /!/ rscsssiiiisrsK sssisiiitsissrssssssssssiissssiiK Sssnssrnccs |H ||H S |5 S S S S ss5 5 ssssss I i| | I KK III ;! i M< HSCSSSSS. 3 3 338S8333S S 3 33 3S 33 3 38 3 3333333 f Hsssssssssi^ik^si^ggggggggbgggggbgsggggksggbg^ggigygsgggysg^ SlesrHssrsSailllltSsSElllliicssIsSsisSeEisESftasssiisSlsgsIssssisssstil i ? 8 5 P w ,, r |5? 5 i l i l . 5 . H ? i i i i ^ ...........t i S H S s s ................ t i335SC3SStSSS3S33S:SSS3SSSSSSC:3S33SS33SSS3SSSS33kS3i:sSStSS33SSs' S S -iiS .ii S 3 S3 i, i CC..S31 ! ! fS S S S S S S B S S 5S 5 t S :S 5 S K K S S S 5 S S S S S S 5 5 K 5 rE B S 5 ..^. t 8 IsIhsIsSHsIIIIsIsIsIIIsHsIIIsIsssIssIsISeHsIIhIIbSssSsS? i 2 S * P B - - . i ^ . e . S B S I i . 8 . i s H . . J . H. S ............. I s s s H s S S 5 =SrSSS3t:tSSSBSS5!;S5j:SbaSS3SBi:8?SSSSSSSS!SissSt c s - iiiis s s t s c -.iis s I f I /(tin t M n win" mm a* J W W kJ U II M/ UI ^ VI MWU ooooooeoooooaooi iiW iw i>iU M taw i*iiiiiiE w l m m 33 *m pm CUMCCi El >uoaau ani t . .SSS HiRRRHilH o s s i i7 eaoslis<e s uo t MM M M i*SmSl* mS Sm mS ue Mo wSWmWwWmWm HR# 5 SSjSS SSSSSS liwu.t. wwa w52Z o o b S o o s S o S S 8 l l S i* S f ]. ???? o l . i i s j ? -: " !f ?$$$$ J * ? i iiw? gf s w2 ? ? !m? ?w? ?s* m l l l p i i 3 -S*"' B i = * lm K m ' bj | j | j | J j j j j j b if fili -es s Ijiji S>11111 I m >H,, eEEGE -----CSC -- B-- - I c i - .sH..sS..sS..sS...>._.........s........ eses: es: S3: 8 ii 8 8 8 8 8 8 !l I " li 1 ipil mn} Fs*: mis::: ;! HH i l|< Hi i B fio a o o o o eooeo J>44IdW *MMWM*4 < O er*m Sm! Coo8ggSo8 *--.-SW---wW--SM--8M----- *o4a a<R#**oo<a oRo e0> %%%%%%%%% n i m m mm *4RMRRMHWMHMURRM MMR %n u n MW MMHM*44UMWWHMROMi RRHMWHh RfIhIKRRPHRRROORRHHHRHHHHHBWRHWHUhHRr m m rm m m i *B f RRR O0WU>-O < 9iutUy ctVibvulM iwnn, rae U w r , *y l t <, M i n i " > <<*- * / U / l e u 0 2 0 1 )1 : g u a t l U M I M f r i M M toy 1m TQMaxMu&st-ymU UHk nm rl, wteMr px mt 4, m w i ad 4m* m . m/U/ , IM, 2 ewp 0301SS( a u t IO ad Md prlMad kr laa I f / l l / t S e U te u w M | r t r o i i O - n t U w , d r > . M t n l u d u t- J > ] OW ( t i l l B M M ilM Md rU tM tqp U i U / U / l l TftMouBtUs-fymca tUtwmicw, Or1pa4rt t. ;rol iad Om * a n . ig/is/st Compound 4 name: IS (Ch4) Response Factor. 1542.30 Response type: External Std, Area Curve type: RF 1.67e3n Tag* I `X>< X XKX aoilti I M U U M I M d prl>t4 ky i*a U /il/ll Kitted lip e rt M th e d LX* : U i t ao d ifiad : P riatad : C : \KJISS l.Y M X \* o u p -rata, p r o V M athM M O lS O O a.adb Non O ct IS Q t i d l t l l 1* i t pcjw ia n Noo O ct IS 0 7 t4 tS l 1M 0 CUiiu^ nmmill %i imml.:i Q uantify Troc*: Coac. *E ItIM U fd l: VOma*ir tHf tkV aFluaacttor: X R ( g t M Window P a c to r i Q tfo a ito T ia * * * window: POAA ( O il) (No m ] TIC Co m . A 1.000000. C iaab lad 21..0000000 0 0 l.OOOODa le tta tiM T iM la tn i): M la c iv * S a ta a tio a Tim *T M t l t u c i : T ia o Window ( o i o a ) i Soak S a la c tio o itoMipp ioMa iiirTyp* 7 .1 3 !. tnablod 0 .0 0 0 . D iaatolad 0 .3 5 N oarast O olyeeaial Typo: P o in t a f O rLolot P it N lglltiw ri A xis T raaaC oroatioo: D ait*i M *)(-te-p**k w w U tu d : Sm oothing: Window a i t * Ik m i I : WvmMr o f a e o t h i i n o th in g a itto d i L in a r Sw cluda 1/Z NOM it taab lad 3 1 J o ia w allay th ro a h a ld : Undue* poak t a i l i n g r R aia* b a a a lia * n i a : S Draw w a rc x c a l ttu ra a h a ld : D ocact ahow ldara; S houlder tk raah o ld : X ilitiv M ig h t: A bM lut* M ig h t: M L ativ* araai A baalut* a ra a ; 3 0 .0 0 3s.0o0o.0 0 > 0.00 O ioahlod 3 0 .0 0 1 .5 0 . O isahiod 0 .0 0 . D iaohlad 3 .0 0 . D iaahlod 0 .0 0 , D iaahlod 77 7 Method M p atc Hothod t l U : UC nodiid: C aveund: P rint*: C: \HA^SLyvx\*au^'rftUi.pra\HthO*M0139>.adb M Oct II 0(>41i21 IIH 2< p r o s (CU2l Rea O c t 1 044:S1 I t COOQUmadMil XMnt lUf. : CwnkKitT r a a i C aac. o{ Kindwaii Oaor IP V alu; Oar M k P accar: (a c c o ra ta Hindoo fa c to r : C h r o M ta g r ta a a indo.* Iks (Ch2) IVON) TIC Cane. 1.000000. D iaablod i.o o o o o o 2.100 1.0000D te to a tio n T ina < a ia a ): ftolotivo IM taatlaa T ia i: RT l l t l f M C l : T in a Miadaw In in * } : Poak S a la c tio n : 7 .3 1 2 , Raaablod 0.000. D iaahlad (H an o i 0 .4 0 0 H uargot haapoaa typo: MlpOMI b ta ra a l knot P o iy n m ial Typa: P o in t a t O rig in : P ie H aiohtiag: JW ia T ro n a C o m a tio a : C aica: 1 in aar te la d o UX P oak-to-paak a a p litu d a : P aoething: Window a i t a 4 c a n a ) : D unbar 1 am>thi: Bathingn a tb o d t 4 E aa h lo d 2 1 Jo in v a lla y chrahaldt I duc* paak ta ilin g : k a ia a U l l U f l i Maxianja: 3 0 .0 0 2 0 0 .0 0 5 .0 0 Draw T a r t i c a i th r a a b o ld : D atact ahm uldarat Shoulder tturaahold: R elativa h aig h t; A haeluta b aio b ti R alativa araa: A bsolute a ra a : 9 0 .0 0 D iaablod 2 0 .0 0 1.S0. D iaablod 0 .00, D iaablod 3 .0 0 . D iaablod 0 .0 0 . D iaablod 1 2It I it ll P Mi* l i *d - i - 11 2 2J 5 i,, mM ! un-.j: ij*jl2>* h ;it |h H tall ills II m 1 Si *. -! IS jI g. J* M -4* SS 3 iS * ! * m3 : ii si lis? HMi-*!w S 3 . 3` itti si li II I !jl .ii llil i H i r n 's i In mi l3'ialoia iiii il '- , JJ5 mi s iti sili s ? i! m # lai f ? le 22 =2 i mi mi rrs iff hs lili i. If fi |i| rsrr :\ l|? E rr fl ? ci" rf 5 Hr* h a e nenn *? i f r -2? ilh .*E<&l ! ft [ H i!! i!f ? i -| jr! !fl` Is s HS *HEB . F r s r? s s I ^ i\ \ m ** ' n f i- M S H % i Quattro C, 6414E SOUP 020199: FACT Equipment Log 99092 PAGE V I PATE:_lflai/39 ANALYSTS STUDY NUMBER: TOX14S MATRIX: ElJivLDESCRiFnONitoiI&4 FACTMethod: ETS-8-7.0 Injection volume: 10 uL Cycle time: 10 min. Electrode:Z-Sprav_____ MobUe Phase: (A)2-Q mM MK4CH3CB (B )J d sQ E ____ TN-A- or sordid number (A) 99Q85::lfl=S________ Prepared (date/by): <M KV10/99 sah_______ (B) TN-A-2878 Expires: (A) 04/00_____________ (BL2fil2_ Store at room temp? @ or N Other: Guard column: None________________ Pan number:jh ________ Lot number: na Analytical column. Keystone Betasil_________________________________ Size: 2 x 50 mm_______________ Type:_JL8__________ Sphere size: 5 um Part number: 055-701-2_________ Lot number: P9E11 Serial numbcr:0591804Z Analytical parameters: Drying gas (L/hr): 350 ESI nebulizing gas (L/hr) 13 LC Flow rate: 100 ul /min. Back pressure: 65 bar Sheath gas (L/hr)JJ____ I1PLC solvent gradient: l(hnia-10-9S Time (min.) QJLflQ________ 2) J U S L _ _ _ 3) 5.50 4) 7 5 0 5LLQ________ %B JLQ JM 2 1S l 25JL 1M_ Tuning Method Report M othod: C : \KJLSSLYNX\SOtTP-RATS. PRO \A CQO D B\PraS3 P rin te d : F r l O ct IS 1 1 :4 2 :3 3 1999 Page 1 MS SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. KS2 Set RdWc 3.00 40 5 0.2 150 250 3.00 -41 -6 153 250 Pressures Analyser Vacuum Gas Cell Rdfak 6.6e-5 4.1e-3 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier KS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Ramp Lens B Lens 9 Multiplier Set RdJbk 14.0 14.0 0.9 0.0 4 650 3 Sat Rdbk 14.0 14.0 10 2.0 0.0 40 0 650 7 38 -0 te; ciMaiiunMa<aiM.iM Lut itoiltiMli Tri et 15UiMil) 1099 r r i Oc* 15 U 1 U 1 U 1M Salame Salar ( mlmm1 0.00 Ometta* t 1 n ME1NlMPair {or- ) Cotar Oham Dalay <1Baca ) t 0.01 Spai ( Daleam1 i 0.00 Start Tiaa ( Kiaa ] i 0.00 Ba4Tiaa <Kim) ; Oapaata i duomi Paraat 10.00 Daugfccar 1 duali (Baca) Cali Bnarvy lavi COM( V 1 11.00 141.00 0.10 10 15 1rmctlm i 2 m OS Urna fair ( UT- Zatar Ckanml Dalay (!Baca ) ; 0.01 1 ,StptMart(tDmaltaimKiaai) 0.00 0.00 K4 Tm | KlM1* 10.00 VSapaata : Qiaaml Parme Daupbtar 1 Ovali Baca) Coll Daargy aV> COM( 1 499.00 99.00 0.10 S *0 s 1 - >MM 1 I M I M U r c 1 I K i r t t Miw l D s la y ( I m i i l . l ) *& t D t i u M > ii s.o S ta r e T m ( M ina > i .OS od T iaa ( M ina ) i 10.0 tip iic a i l duomi trut Pmgfatar tu li {Sarai Coll Bmiw (VI 91.00 71.00 0.3 45 rta o tlo a i l 1 I i riir ( i ir- ) lo c a r C in o m i O alay ( Saea > t Spali { D a lte m I > S t a r t T m ( M iai I i Snd T m ( M ina I r M p aits : d u o m i P arine O auohtir 1 427.0 S0.0O 0 .0 1 0 .0 0 .0 0 1 0 .0 0 1 O vali 0.10 (S ani C oll r i w chnd M port aukUuxi ril: U C Wodifiad FrioCad: cixaakssLinxNSOOF-iuss.FaoNacgBDauoaiA-lo-fs Friday, Oecabar 15, 1999 U U ) i 0 4 Friday, Octobar 15, 1999 UiiJtXS R91100 LC Fusp 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 K V 1100 LC t u r n O n d l a s t t i a a t a f a l The gradient Timetable contains 5 entries which are : Time 0.00 1.00 5.50 7.50 6.00 A% 90.0 90.0 5.0 5.0 90.0 Bt 10.0 10.0 95.0 95.0 10.0 C% D% 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 Plow 0.300 0.300 0.300 0.300 0.300 HF1100 LC Funp xtaraal grant Timetable The Timetable contains 3 entries which are : Time Initial 0.00 0.10 Column Switch Contactl Off Off Off on Off Off Concact2 Off On Off Contaet3 Off Off Off Contact4 Off On Off KF1100 tatoiwpltr Initial Conditions Draw Speed Eject Speed (yl/min) Draw Position (an) Stop Time (mins) Injection Volume(yl) Vial Number 200.0 200 0.00 9.00 5.0 91 1 Pressure 400 400 400 400 400 Masslynx - Sample List Sample Lisi: C:\MASSLYNX\soup-rats-pfo\SampleDB\101599a.SPL Printed: Fri Oct IS 11:56:25 1999 Paga 1 Page Position: (1, 1) File Name File Text MS File 1 101599001 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 2 101599002 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 3 101599003 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 4 101599004 TOX145, RBL10139-H2O Blank-11, SEE 10MIN-PFOS-POAA-PFOSA-IS 5 101599005 TOX145.RBL10139-Liver Blank-11, SEE lOMIN-PFOS-POAA-PFOSA-IS 6 101599006 TOX145, RBL10139-5ppt>-11, SEE 10MIN-PFOS-POAA-PFOSA-IS 7 101599007 TOX145, RBL10139*10ppb-11, SEE 10MIN-PFOS-POAA-PFOSA-IS 8 101599008 TOX145.RBL10139-25ppb-11.SEE 10MIN-PFOS-POAA-PFOSA-IS 9 101599009 TOX145.RBL10139-50ppb-11.SEE lOMIN-PFOS-POAA-PFOSA-IS 10 101599010 TOX145, RBL10139-100ppb-11, SEE lOMIN-PFOS-POAA-PFOSA-IS 11 101599011 TOX145.RBL10139-250ppb-11.SEE lOMIN-PFOS-POAA-PFOSA-IS 12 101599012 TOX145.RBL10139-500ppb-11.SEE lOMIN-PFOS-POAA-PFOSA-IS 13 101599013 TOX145.RBL10139-750ppb-11.SEE lOMIN-PFOS-POAA-PFOSA-IS 14 101599014 TOX145.RBL10139-1000ppb-11.SEE lOMIN-PFOS-POAA-PFOSA-IS 15 101599015 MeOH Blank lOMIN-PFOS-POAA-PFOSA-IS 16 101599016 TOX145. RTL-9R03230M, Dyl. Control- SEE 10/13/99 10MIN-PFOS-POAA-PFOSA-IS 17 101599017 TOX145, RTL-9R03231M. Dyl. Control- SEE 10/13/99 lOMIN-PFOS-POAA-PFOSA-IS 18 101599018 TOX145, RTL-9R03232M, Dyl, Control- SEE 10/13/99 lOMIN-PFOS-POAA-PFOSA-IS 19 101599019 TOX145, RTL-9R03233M. Dyl. Control- SEE 10/13/99 lOMIN-PFOS-POAA-PFOSA-IS 20 101599020 TOX145, RTL-9R03234M, Dyl. Control- SEE 10/13/99 lOMIN-PFOS-POAA-PFOSA-IS 21 101599021 TOX145, RBL10139-250ppb-CCV-11-1, SEE lOMIN-PFOS-POAA-PFOSA-IS 22 101599022 MeOHBlank lOMIN-PFOS-POAA-PFOSA-IS 23 101599023 TOX145, RTL-9R03235M. Dy4, Control- SEE 10/13/99 lOMIN-PFOS-POAA-PFOSA-IS 24 101599024 TOX145. RTL-9R03236M, Dy4, Control- SEE 10/1399 lOMIN-PFOS-POAA-PFOSA-IS 25 101599025 TOX145. RTL-9R03237M, Dy4. Control- SEE 10/13/99 10MIN-PFOS-POAA-PFOSA-IS 26 101599026 TOX145, RTL-9R03238M, Dy4, Control- SEE 10/13/99 10MIN-PFOS-POAA-PFOSA-IS 27 101599027 TOX145. RTL-9R03239M, Dy4. Control- SEE 10/13/99 lOMIN-PFOS-POAA-PFOSA-IS 28 101599028 TOX145, RBL10139-250ppb-CCV-11-2, SEE lOMIN-PFOS-POAA-PFOSA-IS 29 101599029 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 30 101599030 TOX145,9R03230M, Dyl, Control-250pb-MS-11 lOMIN-PFOS-POAA-PFOSA-IS 31 101599031 TOX145.9R03230M, Dy1, Control-250pb-MSD-11 lOMIN-PFOS-POAA-PFOSA-IS 32 101599032 TOX14S, 9R03235M, Dy4, Control-250pb-MS-12 lOMIN-PFOS-POAA-PFOSA-IS 33 101599033 TOX145.9R03235M, Dy4, Control-250pb-MSD-12 10MIN-PFOS-POAA-PFOSA-IS 34 101599034 TOX145, RTL-9R03245M. Dy1.5mg/kg- SEE 10/13/99 10MIN-PFOS-POAA-PFOSA-IS 35 101599035 TOX145.RBL10139-250ppb-CCV-11-3.SEE lOMIN-PFOS-POAA-PFOSA-IS 36 101599036 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 37 101599037 TOX145. RBL10139-250ppb-CCV-11-3, SEE lOMIN-PFOS-POAA-PFOSA-IS 38 101599038 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 39 101599039 TOX145.RTL-9R03246M. Dyl. 5mg/kg-SEE 10/13/99 lOMIN-PFOS-POAA-PFOSA-IS 40 101599040 TOX145, RTL-9R03247M, Dyl, 5mg/kg- SEE 10/13/99 10MIN-PFOS-POAA-PFOSA-IS 41 101599041 TOX145, RTL-9R03248M, Dyl, 5mg/kg- SEE HV13/99 10MIN-PFOS-POAA-PFOSA-IS 42 101599042 TOX145.HTL-9R03249M, Dyl, Smg/ko-SEE 10/13/99 lOMIN-PFOS-POAA-PFOSA-IS 43 101599043 TOX145, RTL-9R03250M, Dy4,5mgAcg- SEE 10/13/99 10MIN-PFOS-POAA-PFOSA-IS 44 101599044 TOX145, RBL10139-250ppb-CCV-11-4. SEE 10MIN-PFOS-POAA-PFOSA-IS 45 101599045 MeOH Blank lOMIN-PFOS-POAA-PFOSA-IS 46 101599046 TOX145, R8L10139-250ppb-CCV-11-4. SEE 10MIN-PFOS-PQAA-PFOSA-IS 47 101599047 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 48 101599048 TOX145. RTL-9R03251M. Dy4,5mg/kg- SEE 10/13/99 10MIN-PFOS-POAA-PFOSA-IS 49 101599049 TOX145, RTL-9R032S2M. Dy4, 5mB/kg- SEE 10/13/99 10MIN-RFOSPOAA-PFOSA-IS 50 101599050 TOX145, RTL-9R032S3M. Dy4, 5mg/kQ- SEE 10/13/99 10MIN-PFOSPOAA-PFOSA-IS 51 101599051 TOX145.RTL-9R03254M.Dy4.5mo/kg- SEE 10/13/99 10MIN-PFOSPOAA-PFOSA-IS 52 101599052 TOX145. RBL10139-250ppb-CCV-11-4. SEE 53 101599053 MeOH Blank 54 101599054 TOX145.RBL10139-250ppb-CCV-11-4.SEE 10MIN-PFOSPOAA-PFOSA-IS 10M1N-PFOS-POAA-PFOSA-IS 10MIN-PFOSPOAA-PFOSAIS 55 101599055 MeOH Blank 10MIN-PFOS-POAA-PFOSA4S 56 101599058 TOX145, RBL10139-5ppb-1t, SEE 57 101599057 TOX14S.RBL10139-10ppb-11.SEE 10M1N-PFOSPOAA-PFOSA-IS 10M1N-PFOS-POAAPFOSA-IS 58 101599058 TOX145, RBL10139-25ppb-11, SEE 10MIN-PFOSPOAA-PFOSA-IS 59 101599059 TOX145.RBL10139-50pp6-11.SEE 10MIN-PFOSPOAA-PFOSA-IS Maselynx Sample UH Sample List: C:\MASSLYNX\soup-rals.pro\SampleDBV101599a.SPL Printed: Fri Oct IS 11:56.-25 1999 Inlet File Dottle Inject Volume Sampl Typ Cone A 1 10min-10-95 91 2 10min-10-95 91 3 10min-10-95 91 4 IOmin-10-95 1 5 10min-10-85 2 6 10min-10-S5 3 7 10min-10-95 4 8 10min-t0-95 5 9 t0min-10-95 6 10 10min-10-95 7 11 10min-10-95 a 12 10mln-10-95 9 13 IOmin-10-95 10 14 10min-10-95 11 15 IOmin-10-95 92 16 10min-10-95 12 17 10min-10-95 13 18 IOmin-10-95 14 19 IOmin-10-95 15 20 IOmin-10-95 16 21 IOmin-10-95 36 22 IOmin-10-95 02 23 IOmin-10-95 17 24 10min-10-95 18 25 10mln-10-95 19 26 10min-10-95 20 27 10mln-10-95 21 28 10min-10-95 37 29 10min-10-95 93 30 IOmin-10-95 22 31 IOmin-10-95 23 32 10min-10-95 24 33 10min-10-95 25 34 10min-10-95 26 35 IOmin-10-95 38 36 IOmin-10-95 93 37 10mln-10-95 38 38 10min-10-95 93 39 10min-10-95 27 40 IOmin-10-95 28 41 IOmin-10-95 29 42 IOmin-10-95 30 43 IOmin-10-95 31 44 10min-10-95 39 45 10mln-10-95 94 46 10mln-10-95 39 47 IOmin-10-95 94 48 10min-10-95 32 49 IOmin-10-95 33 50 IOmin-10-95 34 51 10min-tO-95 35 52 10min-10-95 39 S3 IOmin-10-95 95 54 10min-10-95 39 55 10min-10-95 95 58 10min-10-95 3 57 10min-10-95 4 58 10min-10-95 5 59 10min-10-95 a 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 -- to.ooo -- 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 -- -- -- -- -- ---- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- -- Paga 2 Page Position: (2,1) Maaslynx Sample U it Sample Lis): C:\MASSL.YNX\soup-rats.pro\SainpleDBV101599a.SPL Printed: Fri Oct 15 11:56:26 1999 Page 3 Page Position; (1,2) File Name File Text 60 101599060 TOX145, RBL10139-100ppb-11, SEE 61 101599061 TOX145, RBL10139-250ppb-11. SEE 62 101599062 TOX145, RBL10139-500ppt>-11. SEE 63 101599063 TOX145, RBL10139-750ppb-11, SEE 64 101599064 TOX145, RBL10139-1000ppb-11, SEE MS File 10MIN-PFOS-POAA-PFOSA-IS 1OMIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS 10MIN-PFOS-POAA-PFOSA-IS Maealynx - Sample U st Sample Ust: C:\MASSLYNX\soup-rats.pro\SampleDBM01599a.SPL Printed: Fri Oct 15 11:56:26 1999 Inlet File Bottle Infect Volume Sample Type Cone A 60 10min-1O-95 7 61 10min-10-95 8 62 10min-10-95 9 63 1 Omin-10-95 10 64 10min-10-95 11 10.000 10.000 -- 10.000 -- 10.000 -- 10.000 -- -- -- -- -- -- Page 4 Page Position: (2,2) Dale: Data Analyst: FACT Study#: Matrix/Timepotnu: Sample List' Set-up Analysis D ale/A nalyse Instrum ent: (Analyte: I h & - FACT: DATA REVIEWSUMMARY FORM DU Review Sign-Off - Analyst Review Kme/Date: fY cc k / < / h r(l & X l*\ QualityAaaurmnc* Review Name/ Dele:__________ j y C r/9 -9 y Data Entry: _ U c t& h ilq q Com m enta / Jiu t/lca tto iu : Q . w e /M ( . ^ . ^ p Q iit L - S> m e u t- 'u ja j& n r/t> 7'-. (l o o . YQ ir^ _ A - O E -Calibration C heeks: E xtractio n B l in k E jjC & Q M atrix B lin k : c 'k c o L M S /M S D :_______________ O k (Data Status//) BnltrA Uc to/SU'H IAnalyte: jA cccpU ble L inear R ange: -Y ,9 3 - E y S '. p E ______ ____ LOQ RA2: ^ ~ E xtractedB lank M atrix Blank: Calibration Checks: / 9 A f M S /M S D :_________________ O K ___________________________ _ _ _ Dita Statua/^) Enkrtcj. LAC- |p U,|*h Cg ) P m \*>4S A/p-r- ,J 77A ? Oa i iA 7Tj^> gwaiIT /S e t* * * ? P O M tnfd-i /um7* Chr^P-hiSi^. 7 ? ,fi,, J flfitr tS fi- f - TZt e e - r . j i c sfUf T r ' / v e r / #!&>,A f - G) n s r r _____ fa*r77>,*S JZJTTzeM t t- s-7%i~ M * k .------ wP i<7. <Xui`S v r * r ^ \ i n /f* J .t t r Z fe /y a t- 2 lAnalyte: Acceptable L inear Range: L O Q :. R A2 : ExtractedBlank: _ Matrix Blank Calibration C h eck e IM S/M SD: Data Salua: & M M l T d i t i s S t" Z FACT: DATA REVIEW SUMMARY FORM ?*U- Date: D U Analyst: /0 - o 9 ^ Data Review Sign-OfT A rJ& y FACT Study#: M atnx/Ttm epoinU : Surpl l is t ___/ J / 5 7 .J ? m Name/Dale: fixEtr U 1 o 2- U C O ^/jlj^ Quality A m niK t Review Nem e/Due:______________________ _______________ ssar Instrument .M V * * 1 r } / / ^ . / O fh W Deta Entry;__________ lC- l o / c^ i - l *?*}_____ ~7 I s 0s I I S l S I !o HSS's S s H S ^ iS sIi s3 s ffiS iS a& S S siSiiSS25iif n r r r ^ T r m n h m m r m n ? ^ f fi SSSSSSS88S8SI5S8S5!iSSSSSSStgS8SS8? . s i s i s sstr.^ll f f i i m I j I l l l l l l l 555? H i l l ? 111??? I l l l l l l l l l l h I 3S5????.. SSSgSSS! ?g s i ! 5S3S2S95SSHSSSS8SSSSSSSSSisE2S53SSSS3S lliS lS S sssS S slI.Illilig lilsissss H ;;.^r-oS ioS ;E g5= iss5.oo..f S8 8 B B e8 B S S 8 8 iS S S S 8 5 S !S S 8 * S S K i I Tt T3 ' " ' 2 " " 7 7 7 1 7 7 7 7 7 S g ' ? ? 8 ? 2 3 " ? 8 1 S SS i i S S S S S isatis l i S i i S i S i l i S i l i .ssss assssx sssssu rssskzses I * '* < ' * * 0 * o o o o o m o a 9 e o > n 0 0>< >9 ^ I ^S5 5SSS25 SSSSS SR255 SSRSRSSSS C i 4 s iji 2 l i n ? !!!!!!!!!!! !!!!!! !!!!!! !!!!!!!!!!! 552S25555 ; ! !!!!?*" ! ! illi i!ff J l! im 5 i lpl l!fli! f !i jl^ i U B IS I! i i S iiiiil jl l i g i i I ilililliiiiiiiiil11liiiiiiilii \jm m u um m u uumm !l S 5 2 2 2 2 l|S |iia |S |||s |||n i||||||3 ||i J! l l l l l l l l l `253222ES5Ss3S5S5!;SSSSasSaSSS 1 J i I S S S - - ? 7 2 S S S S S S? | ? = 7 2 * - ? T 9 5 i ssssss 22222222222 322222 322222222222222222 im im i is iiiiiiss sssa5 ssslS ; ssftss IsS Isisissiisssss ! !!!!?!?!? ? 5 5!?5!s!5! ! i llllilllliP P 9?5sgg933? >, 5" ? a ss imi " bbs: mg ^ a * aag sg gg:; ! ||ll S ! ||| sffihsssi H.-J miti sBihS!! l i l i i ili I l i U M U iti U I Iliiiiiiiiiiiliiiiiiiii iil iiiiiiii * fliillllillllliliiilfliliililiiliill 2222222222222222222*222^ 1 :=22:2:SS:SSK22S2S252SS5SSSSR 0 1 ! K 1 3 3 m 1 CMutify CaUknttM i^ irt Tm H i t Dvr ** Compound i uameTTFOS Coefficient of 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 10/ao/MJ w a ll* O C M N i Q w t U t t t o d * r r l a u d b f m O aM Ufy b i U m u w f r t TM 14: M y 1,4 iCompoiw igname: PfO SA Coefficient o f Determination: 0.997888 ' *# 3 ~" ~ /M /W (KiMitify biU knU M ItafMt TM 141 TMjjj&tyT y* " "*"*t,i____ Compound 3 name; POAA Response Factor 33.2811 Response type: External Std, Area Curve type: RF Hf* 1 m il * M 3M s a n t t u m w 4 m k u t f h y a * M /U /W OTmu M1t4USyi CuttU ik mr t UrMBUKttiaf Mwtn. tey 1,< Compound ^ n a m t: IS (Chi) *11MH: OmmuuM m*tmatadtoy 10 / 3 0 / 9 9 p(O i|ilM c u e d ftf SS Oto c-c :t: sss oovvoe IaUi toI Jo in v o llo y tiiraabold: ftodoco poaft talli*: 111 ! i n M i s l . i '? 7 It fi?s 4 : n i i:f i V V * h* s a ^?* 7S3jjSSSS ?S ? :il st: tit 3O r |? * - a*< SU n m I E' * IIP S S ! ?" s5i FB c f. !1 I r 7 i si 8 I Z i l* 0 fe8 < 1 I s MCM4It9rt M ethod r i l e : Lent a o d ltled : Compound: P rinted: M :\aa*U -rt*.P R O \M eeiU \2019f.adb bed O ct 20 O liK M I i n i C 3: M U The O ct 21 1 3 :1 3 :1 0 If* CawovAd wane: In tern et R ef.: Q uantify Trace: Cone, o f Standard: U s e r RF V a lu e : U i r Peak F acto r: I n t e g r a t e Window r e c t o r : C k r o u t t f r i a i m i window: Peak Location R eten tio n T ine In in a ): R e la tiv e R eten tio n T ine: RT R e f e r e n c e : Ti m Window i n l n a t : Response Reaponae Type: Reaponae: C a lib r a tie n Curve* P o ly n ealal Type: P oint of O rlfin ; F i t R olpK ctn: A xle T ro n afo n w tlo n : C oneenctatien U nica: W otH Foa(~ to-peak a n p litu d e : snootn S noethine: Window s i t e ( s c a n s ! ; Munder o f sn o etk o : SnoetR lnp ootbod: latelin es Join v a lle y thraahold: Reduce peak ta llln : R a ise b a s e lin e mexiauw: Peak S eoaratlon Orsw v o r t i c a l th r e s h o ld : D etect shoulder*: Shoulder th resh o ld : R asoense Threshold R elative height: A bsolute he*eht: R elative area: R esolute area: PORA (Monel TIC Fixed 1.008000. D isabled X .000 0 0 0 2 .0 0 0 2. 00000a . 8 7 , Enabled 0.000. D isabled IMonel 0.338 n e a re st e x te rn a l A rea* Llw ear L sclode in done P4 E n a b le d 2 1 3 0 .0 0 2 0 0 .0 0 S .0 0 P0.P0 D isabled 3 0 .0 0 1.50. D isabled 0 .0 0 . D iao blad 2 .0 8 . D isabled 8 .0 0 . D isabled rit< ) lMC N:\M M lie-reU .r0\NUUnVtei9>a.adb ite* Oct 19 asS%Z}Z :sss : t z s Si S*; fi fili! i "SI ii== S3S s>: S so s ia i i e i: t k 3a # u fi HI :s;! sjll Zs s i: . SSSSi ssS lisi2. Hi ! 1 S ,,- ili? j l imsim S a io oe e4oo S3S ! ! III IIIco li jMeMSW>e***S--k*i*+Seuni*iuueym l: i l z i M a ?S| S..J :i!55J II f HHii P i! S S : ; ; . ` s21s 3|ee l i s i s i :K. uS s3USe* -9* S9-* s e S ii* Nette* f il : Lese editi*: '''. AMELIA 062498: FACT Equipment Log .99114 Quattro , 46448E PAGE DATE: 10/19/99 ANALYST: mmh STUDY NUMBER:TOX145 MATRIX: ratUver DESCRIPTION: dii FACT Method: ETS-8-7.0 Injection volume: 10 uL Cycle time: 10 min. Electrode: Z-Spray Mobile Phase: (A12.0 tnM NH4CH3CQ2 (B)MeOH TN-A- or itndid number (A) 99085-10-14 (B) TN-A-2997 Prepared (date/by): (A) 10/16/99 sah (B) 10/16/99 sah Expires: (A) 04/00 (B) 04/00 Store at room team? (Y| or N O ther Guard column: None Part number: na Lot number na Analytical column: Keystone Betasil Size: 2 x 50 mm Type: C18 Part number. 055-701-2 Lot number P9E11 Sphere size: 5 urn Serial number0591816Z Analytical param eters: Drying gas (L/hr): 300 ESI nebulizing gas (L/hr) 10 LC Flow rate: 300 uL/min. Backpressure: 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 T u n in g M ethod R e p o rt Method : C :\MASSLNX\AMEI.IA-RA.TS.PRO\ACQUDB\PFOSl -6KV Printed: T u e 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 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier Pressures Analyser Vacuum Gas Cell Rdbk 1.2e-4 4.6e-3 MS2 LM Resolution MM 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 M M M itf Method D eport M*tn*d: c:\muixu\Jmxjjk-un.rm\jiCQUB\ima-rrQP-PCM h-ll-rttM A u * t t t a d U u d : Men O ct n 0 0 ;2 3 : 1 1 m * raftU it: TV* O c t I I IIM U k v M t D aley I c l M i NM U4M : 1 MM o f 1 Mm * P a ir ( U P - ) i n t e r Qv m m I D a le y ( Sk i I r Speri I D elton a > r s t a r t Tim i I h i m I : end TIM i Kino ) : fcepeaCa : Chennai Parent Oaufhtar 0.0) 0.00 0.00 10.00 1 **11 IXeeal Coll tflirfy <*V) 11).0 UI.00 0 .3 0 30 Co m 15 IV) Pw cuw : 3 M M o t 3 n h i Mur I up- ) In ter Channel D elay I to c * I : Spec t D alton* } : Start I u h t m a* I i End Tin* i M ins J : hapeata : Channel Parent U a h c it 0.) 0.00 01.00.000 l D u o li ISec*) C o ll U a r i y |#V) 1 4 P * .BO M .M 0 .3 0 * 45 Con* ( V > *o funotlen i 3 MM o f 1 Mere P a ir { 10* i In ter C kam al D elay t Sec* ) : Spin t D eltona I i S t a r t Ti m I K in* ) t en d TIB* ( Mina 1 : Sepeata : Channel P arent Dawynter 0 .0 3 0 .0 0 0 .0 0 1 0 .0 0 t D w ell {Sac) C oll IM erey t*V) l 4 1 1 .0 0 SO.0 0 0 .3 0 40 COBO ( V ) so function t 4 MM o f 1 M m M ir I U P - 2 In ter Channel D elay | See* > : Span | D alton* ) : S t a r t T ina ( Mina I ; End Tina I Min* t : hapeata : Channel Parent Daufhter 0 .0 ) 0 .0 0 0 .0 0 1 0 . SO 1 D w ell tSaca) c o ll ta a r ty lav) 4*S.0O 1 4 .0 0 .4 0 Cone ( V 1 SO Maeslynx - Sampia Uet Sample List C:\MASSLYNX\amelia-raU.PRO\SampleDB\101999a.SPL Printed: Tua Oct 19 14:10271999 Page 1 Page Position: (1, 1) File Name File Text MS File 1 101999001 MeOH lOMIN-PFOSPOAA-IS-PFOSA 2 101999002 MeOH 10MIN-PFOS-PQAA-IS-PFOSA 3 101999003 Tox 145: RBL10139-H2O Wk-11, Ext SEE 10-13-99 10MIN-PFOS-POAA-IS-PFOSA 4 101999004 Tox 145: RBL10139-UverWk-11, Ext SEE 10-13-99 lOMIN-PFOS-POAA-IS-PFOSA 65 101999005 Tox 145: RBL10139-5 ppb-11. Ext SEE 10-13-99 101999006 Tox 145: RBL10139-1Q ppb-11, Ext SEE 10-13-99 lOMIN-PFOS-POAA-tS-PFOSA lOMIN-PFOSPOAA-ISPFOSA 7 101999007 Tox 145: RBL10139-25 ppb-11. Ext SEE 10-13-99 iomin-pfo s-pqaa-is -pfosa 8 101999008 Tox 145: RBL1013S50 ppb-11, Ex! SEE 10-13-99 lOMIN-PFOS-POAA-IS-PFOSA S 101999009 Tox 145: RBL10139-100 ppb-11, Ext SEE 10-13-99 lOMIN-PFOS-POAA-tS-PFOSA 10 101999010 Tax 145: RBL10139-2S0 ppb-11. Ext SEE 10-13-99 10MIN-PFOSPOAA-IS-PFOSA 11 101999011 Tox 145: RBL10139-500ppb-11. ExtSEE 10-13-99 10MIN-PFOS-POAA-ISPFOSA 12 101999012 Tox 145: RBL10139-750 ppb-11. Ext SEE 10-13-99 10MIN-PFOS-PQAA-ISPFOSA 13 101999013 Tox 145: RBL10139-1000 ppb-11, Ext SEE 10-13-99 lOMIN-PFOSPOAA-IS-PFOSA 14 101999014 MeOH 1OMIN-PFOSPOAA-ISPFOSA 15 101999015 Tox 145:9R03237M, Day 4, Control, 0:100 lOMIN-PFOS-POAA-tS-PFOSA 16 101999016 Tox 145:9R03245M, Day 1.5 mg/kg, D:100 10MIN-PFOS-PQAA-ISPFOSA 17 101999017 Tox 145:9R03246M. Day 1,5 mg/kg, 0:100 lOMIN-PFOSPOAA-IS-PFOSA 18 101999018 Tox 145:9R03247M, Day 1,5 mg/kg. D:100 lOMIN-PFOS-POAA-IS-PFOSA 19 101999019 Tox 145:9R03248M. Day 1,5 mg/kg, 0:100 lOMIN-PFOS-POAA-IS-PFOSA 20 101999020 Tox 145: RBL1013S250 ppb-11-2. Ext SEE 10-13-99 10MIN-PFOS-POAA-ISPFOSA 21 101999021 JUflOH lOMIN-PFOS-POAA-IS-PFOSA 22 101999022 Tox 145:9R03249M, Day 1,5 mg/kg. D:100 lOMIN-PFOSPOAA-IS-PFOSA 23 101999023 Tox 145:9R03251M, Day 4, 5 mg/kg, 0:100 10MIN-PFOSPOAA-ISPFOSA 24 101999024 Tox 145:9R032S2M, Day 4, 5 mg/kg, D:100 lOMIN-PFOSPOAA-IS-PFOSA 25 101999025 Tox 145:9R032S3M, Day 4. 5 mg/kg, 0:100 lOMIN-PFOSPOAA-IS-PFOSA 26 101999026 Tox 145:9R03254M. Day 4,5 mg/kg. D:100 lOMIN-PFOS-POAA-IS-PFOSA 27 101999027 Tox 145: RBL10139-250 ppb-11-1, Ext SEE 10-13-99 lOMIN-PFOS-POAA-IS-PFOSA 28 101999028 MeOH 10MIN-PFOSPOAA-ISPFOSA 29 101999029 Tox 145: RBL10139-H2O blk-11. Ext SEE 10-13-99 lOMIN-PFOSPOAA-ISPFOSA 30 101999030 Tox 145: RBL10139-UverWk-11. Ext SEE 10-13-99 10MIN-PFOSPOAA-ISPFOSA 31 101999031 Tox 145: RBL10139-5 ppb-11. Ext SEE 10-13-99 lOMIN-PFOSPOAA-ISPFOSA 32 101999032 Tox 145: RBL1013S10 ppb-11. Ext SEE 10-13-99 tOMIN-PFOS-POAA-ISPFOSA 33 101999033 Tox 145: R8L10139-2S ppb-11. Ext SEE 10-13-99 lOMIN-PFOSPOAA-ISPFOSA 34 101999034 Tox 145: RBL10139-50 ppb-11, Ext SEE 10-13-99 10MIN-PFOS-POAA-1SPFOSA 35 101999035 Tox 145: R8L10139-100 ppb-11. Ext SEE 10-13-99 lOMIN-PFOSPOAA-ISPFOSA 36 101999036 Tox 145: RBL10139-250 ppb-11, Ext SEE 10-13-99 10MIN-PFOS-POAA-ISPFOSA 37 101999037 Tox 145: RBL10139-500 ppb-11, Ext SEE 10-13-99 lOMIN-PFOSPOAA-ISPFOSA 38 101999038 Tox 145: RBL10139-750ppb-11. Ext SEE 10-13-99 lOMIN-PFOSPOAA-ISPFOSA 39 101999039 Tox 145: RBL10139-1000 ppb-11. Ext SEE 10-13-99 lOMIN-PFOSPOAA-ISPFOSA tu u u u u u w ? ? ? :.................................................................... m sess SSS s f 2 f s f s s fIuDt cI?OnDus?&B$)0t tOf&02S<uO^s3ID?5<&b$<sgbs(ibusU utsti<GOIewDe<tt)*sD3(uDs(<D7Oi w 3?52 I I I II I I I I I II M ! I 1I! I I I li I I I I ! I I I i II f I I M ! i I I il I I I ( i I I I ! ! I I ! M I I M ! ! I I I I I M I I I I! Ml ! I m i l N M I l I M M I I M1 1 I ! II m i g Mill M l! I II M M i I! M I M I II ] I M II I M ! M II II M M M II l i 1 M I M M I M I I 11 I I I I I I I I I I i l M I I I I I I I I ooao m I l 11 M I I I M M 11 M I M I I I I I I I i l M 1 I I I I I M oo3f> TJ v3> I ?s FACT: DATA REVIEW SUMMARY FORM Date: D ata Analyst: *:FA CT Study s f*/S - Mb/v Mjtrix/Timcpoints: -tv e* / U - c J . Sample L ist QZf f f c Set-tip A nalysts D atc/A nalyst j t/*$(?$ Instrum ent A b jt* O it-fn tM J *Mirt: To m feu l iB> [Acceptable L m ear R ange: ILOQ:___ U . f r j j l M = ___O M iftt, L /3oj-t,L - i M f f L Entraction 'Bltnlcjf d r &**L M atrix B U rik ^ r i r a ^ r `tk^-Uxi Calibration C hecks: $ J a 1MSM5D: A DaU Status: Ml A n aly te: 7ZS cn'j Z^O jA c e ep tib le L in ear R an g e: jj ____________ LOO: )2.3SyfS, Extracted B lank r * o .n ^ n z - M atrix B la n k /tes L a UQ f t AC alibration C h cclcc IMS/M SD: M. Data Status: Ml Analyte: ^ w M*(A cceptable L in e a r R an g e: LOQ:___H ---------------- UE x tracted Blank: |R"2-- ......H k ---------------- CalibrationChecks: tfo M S /M S D :___ ID ataS atu s: hIa jo)a M atrix Blank: A /A ? IA L l o M t t D a ta R ev iew S ig n -O ff A nalyst Review Name /O nte: J k s __________ Technical Review N a m e /D m v.^ r Q uality A ssurance Review N o m e / D a t e : _______________ D ata t a i r a Oc Comammeennits /JJustifications: O 1L u s LA lo h l/W *'m~ d ix . -fg -U r -t v _ u ^ A jL c . ra-a-fa. 7 L LT k ~ J _} L - d e v jjx e J /, a id e * ___ - f t g e t a. y * lte ]m - i - teci-c- d t * - -- o-n,.- f.'7ki ..CUVtti, m*/- O/nS Qcfsis/e / ~/Ae ( n t r sL -J -iM - Cukm U . - 7 * .r * /z* /fy /ka- r A * * . <aca-,.?us. -- X * g ^ L f t f ^ toe.* d r e j^ -e d ___ -fi-pt- 4 L OLriML 4, 4 i* .t -/c L-j w Bk b f i j j Lt. /ess L -- 4 L lo g , 7 b - b!$ if kxiAs O ttitid e d /*- r d i v da 7>nUtcL. A. a3d l /,*** , r * M t ia m - C a w - .M (Luid-H ui U+S ^ Ade- -TS h ik e d fa e s ts le id J ^ --diQ tK L d ...a , c/cufad'**- * t &*/. (d u A U tim id i* * - L . (koli* Pik- k So L i . FACT: DATA REVIEW SUMMARY FORM Date: Data A nalyst H:FA C T Study ah *L 1 TV 'S M aihx/TimcpoinU: ~ E Sim ple L t jpZSfy C ____________________________ . U l r & Set-up Analysis DiLa'A n a ly s t Instrum ent .. /o /W /y ^ *A*uJul JH S D aU Review Sign-OfT A i t l j i l Review Huk -N am e / D ate: _ * 2 . T achaleal Review Name/Date:____ M tf.___ k . pty, \fi lAC lo/zlp Quality Assurance Review N a m e / D a t e : _________ Data Retry. Alo e n k ^ (AC io A z M Commenti /JuitU kaU oni:_______________________ 'Z b jjjJi pmis &> 'H * 4 - -fi* ___ ll u t- h V o u M Lm. 'H * .--------- Lod. / b it-* -a * '{f`aSA ______ hKY* -AxLs L h j L -- !>/,h i x .-n * c .-n ^ -J -^> g- <g- p ~> & n u ~ w-5. , /-J-- /03-?/< }9 I i ! S I i ! i * i iSESSsss. J SSSSgBiiSS S rrrrrrrrrrr 555=55=2532 SESSSSi I E.ESS SSSSSIJS fS f||f|S S ? 3 ! s 5=i" ==5=tSs SsKSS 5 5 " I s Cm,, 00? s s e s s s s s s 's * H ****lM i| BO AjT3ii ? I a7ss=--5? 1 sssississsa ii - S-S - S -S S-S-S - j m nm n s iss;Ss55s5s i i : V, 5 i X n i m 1 I isa lh s isss hh r> <* O r o o o <'10*0 iMniotn*n^r*N 4 n "2 ~ o o * * HMN t -o-r<*'ronrr*> fv*r-pf-4in- rr*-*'>- ^vba >. * sssssssss U rio C f.1 3 "* ESSTE m i mili!]!2 S 2 i* iliiiis in ! S 2 .sss;? ? t O SN SH H C IM N i 11 JEooo2S- iis " isU 3 Isis fi ! | 1! m u mN3KitiN*, N in__tM_ _H_lN_Xf_tj_Ht_Ni, S33SSSSSSS3 isiliiliiilii - 3 3 3AAASUA is u3*na ii I l l l l i i i i i i l i Pilii1 1 *>>3tI 3S O o tf io r 'o o O 'jr tn v iA o t- 0O0o O9o O9OO0o O05>O0o O0o 0Om0Oo 0Oo 0O 0*s INNMN^NnnnnnnS #0009000000000 u llhi i i i Ii ! I Q uantify d l i b r t U M i f i n T Q X H 3-rit*ut l l m m - a n . i a / 2 3 / f MW Compound 1 name: POAA (C hi) .Coefficient o f Determination: 0.996986 iCalibration curve: 0.253166 * x + 36.3287 / ` tenia* 9434M: QhmUu M m4 prlnCato toy \n*t\ Quantify C tllb riU M art TO (U 5> tatibU ll * f w r w - M ( . l l / } 2 / l l Compound 2 name: PFOS (C h i) Coefficient o f Determination: 0.992922 Calibration curve: 6.34685 x + 149.692 2 M U M 3 M : 9m U U M p r in ta tl Irf 1m M / 2 I / H O M aU fy C U U k n U M K n 4 S -n M u t U v r oarv** a t. 10 /1 2 /* * *** Compound 3 name: IS (Ch3) 1*9 1 Q M U (y C ilik m io n M p n I Q H I l'tttiU t U tr a i m * u t . 10/33/** Compound 4 name: PFOSA (Ch4) Coefficient o f Determination: 0.996087 Calibration curve: 17.5980 * x + 76.6733 .'Response type: External Std, Area Curve type: Linear, Origin: E xclu d e, W eighting: 1/x, A xis trans: N on e <m I1 i 0 0 0 4 : Q u t a U U U d M l p r U U d b y 1m 1 0 /X C /* * VO-?4 ss K L i l ili :'ljs P U <*b Is 8 s S yK 33 ii - S. J C if! i 13 *$ 2 * .. 3w . wj . >S* ; 3 233 , 3 3 Ji s.-l S l . S -i jjj-t hI I!2J `SS:$T!3 SS J3 s93s ~eHu.i *C Mi*b* rl filili - m *I -l- ee io S*!!' il#*O* -5.j!ec l :*pniT1dB llioMS 1- 5 in; , oi mo o o S1*. SS88 Join * * u r ttirM M U : Mduc p*k _S wX"*imnTaJTs it.-. s2 :. i a::slf?almfsmff m n i: i a --% Hi ms5 s i u o*S * s i 1 apn^tT^at ta d -o i-y a a , IS S n a a IA { ii`1 ni I-ff a a V i- n i?: T*S* r'o if nr S" ?t fi| ni3*4 2 2 : ; E" ; s 3 f; ij on 'i ? *s4i2 ~ fili ill r II"* 5 r SS 3 3 I i: : i t; R3 5?S t* SB aa I 2|? S* ` 3 n n j r a S i na m " Method Report Method f l i t : Lose m odified: Compound: P rinted: C: VMASSLTM tteneUaOSaOa. P * O O te th N U 0 2 3 c .mob Two O ct 3* O f : 9 4 :4 2 l*9C 3: 13 (ChJt Tve O ct 3 MW Compound Marne: U t t r iu l R ef.: Q uantify Trac: Cone, o f Standards: Usar *T Vala: Usar Peak fa c to r : Zncetrace A w fa c to r : Chromatogram mass window: Pea L ocation R etention Tine In ln u : R e la tiv e R eten tio n Tine: RT R e fe r e n c e : T ine Hindoo In in s): Peak S e lectio n : Response R espite# Type: R esp on se: C alib ration Curves Polynom ial Type: P oin t o f O rlffln: Tic H eipbtlA f: A x is Transform ation: C oncentration U nics; H olee Poak-to-poak am plitude: Smooth Sm oothing: window s i z e U c e a s) Humber o f a n o ch e: Sm oothing method: D atelin es Join v a lle y threshold: Reduce peak ta lU n o : R a isa b a s e l i n e maximum; Peak Separation Draw v e r t i c a l t h r e s h o ld : D etect shoulders: Shoulder th resh o ld : R esponse T hreshold R ela tiv e heigh t: A bsolute heigh t: R elative aroe: A bsolute area: IS (CUJI {Hone; TIC fix e d 11..004000000000 , D isa b le d 31..00 00 00 00a .> , enabled 0 . 0 0 0 , O laablod (Poae) o.asi M oaroat Iscsn al broa L inear E x c lu d e 1/ x 71 2E n a b led 3 0 .0 0 3 0 0 .0 0 0.00 D isabled 3 0 .0 0 l.SO , D isabled 0 .0 0 , D isabled 2 .0 0 , D isabled 0 .0 0 , D isabled 3rege i I n; SM V. E 8 0'2 S .1 l SS ! li i il s_ . i l | i | Si s i l i S n 3 a al ia al al ?S -Ssl a f i * si sSi*.l i ! laa- il i 3 -< J D 35 * 4* > M V . -a ai s. :1 sisfl a; l|!x Si?! SSiJ SSiS !6i E Mi tn>>isU53f2Ciwe.oci;l sl *a i s: IsZsi tiSS Ili !i5i! flti su s sis sis JoMomdocv*opUo*yk throsfcoid: ? K xl i m tma ss "` ss; s l s ss 2 usi AMELIA 062498: FACT Equipment Log -99114 Q uattro , #6448E PAGE DATE: 10/25/99 ANALYST: ms STUDY NUMBER: TOMS MATRIX: Rabbit Liver DESCRIPTION: Curve FACT Method: ETS-8-7.0 Injection volume: 10 uL Cycle time: 10 min. Electrode: Z-Spray Mobile Phase: (A )2.0 mM NH4CH3CQ2 TN-A- or stndid number (A) 99085-11-3 (B)MeOH (B) TN-A-2945 Prepared (date/by): (A) 10/21/99 sah______ fB) 10/20/99 ias Expires: (A) 04/00_____________ (B) 04/00 Store at room temp? |Y] or N Other: Guard 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 param eters: 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: 10mtn-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 HLO. T u n in g M ethod R e p o rt Method: C :\MXSSLYHX\AMELIA-RATS. PRO\ACQUDB\PPOS1- 6KV Printed: Mon Oct 25 10:13:58 1999 Page 1 SOURCE ( ESP- ) Capillary Cone Extractor RE 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 Sat 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 46 39 48 L e a t M o d ified : Mon o n I t 0 0 : 2 3 : 0 199* m nUd: Mon O ct I S 1 0 :1 1 :3 1000 M lV M l Dalay in* ) ; 0.00 n M U M : 1 MM i f .Maaa rir |Mr- ) In ca r C ltM M l Da la y I S ac* ] : Span ( p tU a n i I : S ta r t Tin* l Mins I : End T in e ( M ins I i Papeete : Channel Parsec Oeoyhcar 1 413.00 14.00 0 .0 3 0.00 0.00 10.00 3 D w ell (seal co ll Cnery (eV) 0 .3 0 10 rw icU M i a MS4 t 1 Maas K i r 4 I Incar Channel Oalay I Sac | : Span I Dal c o m ) : S t a r t Ti m I Min I : End T l < M ias > : Repeats : Cnsnnal Parent 0euhter 1 499.00 99.00 0 .0 1 0 .0 0 0 .0 0 110.00 D w ell IS a c s! C oll E n erg y ta V J 0 .3 0 4 Co m I V ) 0 P unetie* : ) MM o f 1 M m P a ir ( U P - ) In ter Channel D elay ( S ees > t 0.03 Span ( D altons I : 0 .0 0 S t a r t Twee | Mins > : 0 .0 0 End T ie* ( K in s I : 1 0 .0 0 Repeacs : t Channel Parent DauphCtr D w ell I S a u ! C ell (nervy lo V ) Cone ( V ) l 427.00 0.00 0 .3 0 40 10 VUnctaew : 4 MW o f 1 Masa P e a r I M P * I In tsr Channel Delay ( Saca ) : Span I D altons ) : S t a r t Tana < Mina ) : End T ina t H ina : Repeats ; Channel Parent Oauphcar 494.00 70.00 0 .0 3 0 .0 0 0 .0 0 10.00 I DweLl (Saca) C oll Enaryy (aVI 0.40 U Cone < V ) CO Method Raport Method Pila: last Modified: Printed: c *\maaalyox\ailia-rata.pro\acqudb\lmin-10 -95 Monday, Octobar 25, 1959 10i12>15 Monday, Octobar 25, 1999 10:13:44 Page 1 BPllOO 1C Pump Initial Conditiona Solvents At 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 Let(*C) Oven Tenerature Right(*C> 0.300 10. 0 400 30.0 30.0 BPllOO LC Pump Oradiant TisMtabla The gradient Timetable contains 5 entries which are : Time 0.00 1.00 5.50 7.SO B.00 A% 90.0 90.0 5.0 S.O 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 Pressure 400 400 400 400 400 HP1100 LC Pump External Event Timetable The Timetable contains 3 entries which are : Time Initial 0.00 0.10 Column Switch Contactl Off Off Off On Off Off Contact2 Off On Off Contact3 Off Off Off Contact4 Off On Off HP1100 Autoeampler Initial Conditiona * Draw Speed 200.0 Eject Speed (Rl/min) 200 Draw Position (mm) 0.00 Stop Time (mins) 9.00 Injection Volume(pi) 10.0 Vial Number 13 Masslynx - Sample Uat Sample List: C:\MASSLYNX\ameila-rats.PRO\SampleDBV102S99aSPL Printed: Mon Oct25 10:13:12 1998 Page 1 Page Position: (1.1) File Name File Text MS File Inlet File 1 102599035 MeOH Blank 10MIN-PFOS-POAA-IS-PFOSA IOmin-10-95 2 102599036 MeOH Blank lOMIM-PFOS-POAA-IS-PFOSA 10mkv10-95 3 102599037 T0X145-RBL1Q229-H20 Blank-1,10/22/99 RWW lOMIM-PFOS-POAA-IS-PFOSA 10min-10-95 4 102599038 TOX145-RBL.1Q229-UverBlank-1. 10/22/99 RWW 10MIN-PFOS-PQAA-IS-PFOSA 10min-10-95 5 102599039 TOX145-RBL10229-5ppb-1,10/22/99 RWW 10MIM-PFOS-POAA-IS-PFOSA 10min-10-95 6 102599040 TOX145-RBL10229-12ppb-1.10122/99 RWW 10MIN-PFOS-POAA-IS-PFOSA 10min-10-95 7 102599041 TOX145-RBL10229-30ppb-1.10/22/99 RWW 1M1N-PFOS-POAA-1S-PFOSA 10min-10-95 8 102599042 TOX145-RBL10229-60ppl>-1.10/22/99 RWW 10MIN-PFOS-POAA-IS-PFOSA 10mln-10-95 9 102599043 TOX145-R8L1Q229-12Cppb-1.10/22/99 RWW 1OMIN-PFOS-POAA-IS-PFOSA 10min-10-95 10 102599044 TOX145-RBL10229-300ppb-1,10/22/99 RWW 1OMIN-PFOS-POAA-IS-PFOSA 10min-10-95 11 102599045 TOX145-RBL10229-600ppb-1, 10/22/99 RWW 1OMIN-PFOS-POAA-IS-PFOSA 10mln-10-95 12 102599046 TOX145-RBL10229-900ppt>-1.1002/99 RWW 10MIN-PFOS-POAA-1S-PFOSA 10min-10-95 13 102599047 TOX145-RBL10229-1200ppb-1.1002/99 RWW lOMIM-PFOS-POAA-IS-PFOSA 10min-10-95 Masslynx - Sample L ist Sample List: C:\MASSLYNX\amelia-rals.PRO\SampleDB\102599c.SPt_ Printed: Mon Oct 25 10:13:12 1999 B ottle Inje ct Volum e t 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 Page Position: (2, 1) FA CT: DATA R EV IEW SUMMARY FO RM Date: i'fr tfil Data A nalyst M:FA C T Study T rtm . IvbinxiTim epoinU : ~7ua* Xi~J*se CaufiruS/ Sunpt U * : fO?f99a- ---- Set-up AjuJysis Date/Analyst: "/u fo At& /Zn t f t f n ftL Data Review Sign-Off A nalyst Review . N am e/D ate: 3 S fo ilHi .( o j f j f f [ ( f t Quality Aasarance Review Nam e/Date:____________ D a ta E a tiyc: L t o h N D T ( f f p r j p d * L Instrum ent S 2 A n a ly te : ToA* Q&rtt (Acceptable lin e a r R ange: / 'LOQ:___ l-OOnk RA2: O.ff.'S file-C alib ratio n C h eck a: Extraction Blink: fjA MtM a rrix B la n k Skh~- 12"/" ** M S/M SD: iDtU S tatue C enanaati / Jo sti/k atlo ru : 7C S * - / T ^ z jv L Cunr*- >,*Js jCtm. ft\ . J ,, t 7m/ ft*4*.r -fiff -A J L Curve e.*~ci / it-tp JtVtlcA. a. ~fi L u s a 4 L CU+v*, t4 le s s SCjlu ~ &"% . 7 f/t hr** Aj> aJ j S e^S re^S - e U ( U L 4 L (tV*,___ -- fLi_ y e JJ.L y " U t1 kX re SSraoyStxuSJ L k - S L Cu m . I in /, S> ..5^vrntia d*__ < tjavii / !nua s SSU 4- kep efeo!-/> l**s S L u~- --3o*A /e- S fou*e*< L U J - J L Curve I LmVC tjiv e H,, 9 tS tS f l e a / ___Yu*- u S ls SL* S**yL. A n aly te: DfhS* ( ein')w s r W . - 'f a i n Acceptable Linear Range: LOQ: T s.fo ^L 'Sto Extracted B lank MX R A2: M atrix Blank: / / 4 Calibration Checka: 0 7 L /.W S b ./Q uJr j U s J r - fU LixecrnojmjL*t* . S fo j l * J Jtuia So u.9 Sr* Su :>- - l l l QtlC. S Wcar-e 4 i* ~ 3 o `/>.__ M S/M SD: _ ^ l*j L s kjtre 4 o Jl j L S u*. So____ Data S alue a tu c so J c c y t-e fo ru c -ftt/ 0>~J f/u tJ d Lc. w>tu twf k m f i t e fa /w te n /, DuI > fits rl z p M O tU K U Lfo. f t b r m b iti b in eccuS & fn U O fa tm fo a S fk & i* fk s- v .u l - ti f i f t v FACT: DATA REVIEW SUMMARY FORM Dale: ''J-nfvL Data Analyst %.f a c t study `Toxt'ff M atnx/Tim epotnls: ~Jru Sampk Lot }o7X9a. *?*z/l9 Set-up Ajitfyi Date/Anaiyjt h h i f U l* /I S __________ D ita Review Sign-OfT Annlyta: S CU-*f _________________________ Acceptable L inar Bange /**_______________________ LOQ:______ a _________ Extraction Blank /M RA2 :_______ H A_________ Matrix Blank N * Calibration Check* H *.__________________________ MS/MSD;______________ ' Data Statur:______________ ' '_____________________ __________________ l L /*. -/Le. /a***- e jjc d,* -J h9k> J* -fL sL ___- 7 ^ MX e . r<ax- /L y -}Li- GcCqa/ /r e p * / /j L /J h CoH jx H 'e / *ii*Ct>Jcfiu(A--[r--h~ U/XLS f-b - '>r*I-JXH-IHA & *j L k J k z ___ta a c L . Ir- h H tz d J * . 'ICm j * . & ~j >/ac /J t l* . / e f j c h t c / t J f a . n j h e m * ., 'fk j-g - t6 / X T t S >'>i r i / f 9 ___________________________ n u t i - t m a a 4i* MuCintetiM* r r w / m u ; M M **! u*> Ciaj4i.fxs*Bi*poat.^v --iiwv: mu nnMm:m u u * a : criur teuoscLmaxxwpTeiowaeiasaciamf.FriexjeefcMBUe: u m m o r M B ii i i i M a* o/ao/ im PrlaaWi rrt OCX 3 47:]7i39 1 099 K U <Cte) Umm 1 1020**001 2 1030**003 a 10209*003 A. 1030**004 S 1020*9005 4 1020*9044 7 1030**007 a 1020**000 * 1020*9009 10 1020**010 i l 1020**011 12 10200*012 U 1020**011 14 10209*414 1S 14209*015 24 1*21*9014 17 1424**417 10 1034**414 1* 14249101t 20 14241*030 U 10201*021 32 1020**022 31 1424**021 a 102***424 25 1434*9025 34 10249102 27 102499037 20 1421*9020 2* 10209*02* Om* U U k tM t HON 01k Matt 01k r a O x 't* M -4 )-l, Ippb- 9/10/9 Mtel rCHM-04-41*3. 3te- 9/10/99 MW rO4ix-9044-41-l. 10te- 9/10/9* MW rOi-**Oi*4l-4, M ppt */!*/** MW rCXix-9aC-}-S, 50ppb- 9/10/99 MW PCXLx-*044-43-. 100te- 9/10/* MW rcniji-**oo-3-i. asoppte- /io/** mw fO*ix-*9004-41-1. $M**b- 9/10/0 IM 9CWUI-09004-49-0. 7S0h 9/10/* MW MteOB OU TOUio-iros/foib* u T M i - o m - a w o - 1 0 / 3 /* zas TOXKS-PfOS/PGAA la TteHHte-- -4fte- 10/20/* ZAS fCMia-*004-43-4. 35te- /IO/** W M MhOS 01k roxm-orosA ia m -- .a4pi>- 1 0 / 2 0 / 9 xas TOX34S-rrOSA ia T v c a a ---lOOpteb 10/10/9* ZAS rO4ia-**04-43-7. 234pb 9/10/* MW i m i ak r a i i j i - m i H M . lppl- 9/14/9* MW rCMia-1044-43-2, Sppte- 9/14/99 MW tatix-99004-41-1. lappt- 9/14/99 MW racia-99044-43-4. 25pb- 9/10/99 MW raUx-99044-42-9. SOppte- 9/14/9* MW PCXijr-004-43-l. 100pte- 9/14/9* MW raLU-99444-43-7, 2S*pto- 9/14/ MW rcaia-99444-41-9, 5Q0pte- 9/10/99 MW KXLh- 99044-43-9. TSOppb- 9/14/99 MW ! ItMteur u a lte lUM ittd luteU ro StAWUrS tfa M r StiMUrd lU teU rt Itm U rt OC OC Ifw 0rt CtMOteO ItW rt I c ite lin l itaau n l -- 1-- * iroO iH lu a A v l Standard *d Cmme ar 1.44 5.S3 14.40 25.1 90.20 100.00 351.00 903.00 733.00 39.10 7.043 7.107 7.005 7.007 7.092 7 . OIS 7.110 i.m T.111 7.104 7.114 7.139 7 . U* 391.00 7.111 7.1*4 7.133 1.00 3.03 10.94 33.10 90.30 100.00 331.90 902.99 . 733.99 7.13 7.124 7.130 7.137 7.123 7.110 7.113 7.111 7 . U* Kerne P lan em e. toten 17 IM 30 tote 47 Ml 193 tete 144 bb 741 tete 3710 tete 3905 k U 3991 ItteX t tob 447 tote 41S fato 2 1 m 410 tote 414 Ml 1775 tot 1 IM 4 tob 95 MC 312 tote 422 tote 1 bb 141 tob US bbX 40! toter 0.05 3.09 10.19 24.7 40.04 90.45 240.S3 407.30 541.42 0.00 99.31 55.07 20.10 -15 -ZS -1 -4 -0 -4 -1* -20 11 53.45 97.50 340.01 -4 1.10 4.74 11.41 37.42 54.40 149.94 245.90 421.05 553.0 14 -5 15 9 12 14 -2 -15 -34 * i oh 0301*11 OuMttRtd u4 fflMMl ter Ite i/a*/*t > I ST-TTT' TS 3S5- 3 3 S S is I5 g ;5 S 3 5 3 S | liu im u lim iu m u tm iH l 5 3 lS a g g l5 S p -||| H 3 S 2 H li| i mm I hhshh I n*S! ? II***!!1? M i Hi 1 H i i l l i Owulty C S333JSS53SSSSSSSSKSS j Ss"??7777 5 3 SS35-33-? A fs jp ir a Ul-iI2iIi*IS!Sp*ljii|i||4*pll|8!|j3|i522S| Sp2*s^*.sr?*VShg.`r-5r2rSf3*^5r2-'r2<3S^5f."3S Si*.'3r*5r^K S 3r S- W5Sf*s*' 1 su s ima 1m * i1s i!1ih1!Iih - > * * * * M . liillllll . , iiiiiii J!V V*, lsilslslsls! ips! 14a1 SiSsissis Mllllls i ij|i lllSlisSlililS S i : lie* 2 o S S S C v i x ** * 8SS5 s iiJilf1 lP*bP I;Si?-t* si il ilil 1 ! J H l i l I l i u i l lS 3 3 3 5 3 3 5 5 5 5 S S S S S S S S S I J ! |s ssssasass ' - T rrsaaaass j! 2 3 2 5 5 2 5 5 5 3 5 : 5 5 : 5 5 5555553 El 111111111 111 111 i i i l l i i l l p m u m m m in silili s SS5SSSS35 333 335 533335333 f !. h*h I " ! " *!!! 5 * * SSh > H H ?3 3 liti*!!!! l=i p i ,, m u l i lllffi f i P l uttjtfttjjt jjl iiUS.il saansaaaasssasasxsss ------------------- ----------------------------------------------------------------------------------------------------- r-- j-------- 7------------- O M U llr aa ifcrteiM u i m f o u t S 't M M to 4m M t i n t t k M - r r u / m u ^ o a n . x t m / f t l u ' w* x Compound 1 name: POAA (C h i) Coefficient of Determination: 0.996938 Calibration curve: 7.35186 * x + 10.5814 Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 1/x. Axis trans: None BB m IOIMi mmI priata kr lu OMHNltyCtUbriUM --art W U 4 M W U M 4m -- f i t i r r i -- - r m / i r o u / i o a a m . m / i i / m i m 3 3019*1 iMUlMMd Ml pria*4 toy Im m U/1I/H On uttiu-ilrcaitIett4iMm MgotriBeMiM* noi/vrou/tou *c. /ai/* im XX j fru u ftfr G lu ru iM M |M t * am i*tN M 0 Am M tU a w tU ^ p r o t / m u / f o u *m. 1/1I/I 1a >Ki 4 2 i 3 i 1 > ? S li8 l i 3 iini ll_ fi *** 2 i lisi I! ^ ! o a ~ fc ;1 1 1fi ! 1 li ss 1 ;|i scs 32} ** 1 *' uhs 6i iu Sb Zb!#-9 II isl. i: ; sii' m2t 2*I h*BJ1 pp j3! lisi 1 3* 1 mh .i S S*m ili jss Ili jjl 323s iUi3:fi ? o2 -M iS" J Ufi ili sii i*3 sI>Ma2Ai3 mi m 222a H i. ss * lisi ,J ! i Jo in v*ll*y thcoobold: duc* pk s til in e : un H fl i: itti ilu :a h a ig tu ; I !* a P i & i J] i! i Hi! si M . .s!i i l S" ! r-' : |i ! sW iC iU ;W:bsaI U*3Au BDM0 iill . . 22I2l ?i lfs! zi iJ8 3 !h..S.1 n i I il 3 S? lisi Ifil ii Sij- i*. -js fres 3 *P 3* B r i :Si 4*4B K e S * SS iili 3.3 J as5: IS -o 1 :1 IIlIl! im 1111 oaaa nono AA9 - Ili ? 3 i l 31 Mwtted kpon Mattod <nr UC M dUi4: Coapound: tl tid : C:>MimnXV*v420m.pr*\Mattil\1020t9*.nb f r i ct 239 l :U i) S 1l f*99| 4:; ZS CnOuU) f r i Oet 39 0Tj H ;I J 1*99 Cnfnuml B*mm : In te rn a i MC. : Ouancify Troc*: Cm c . of tcandard*. TJ**r AT Valu* i 0*r N ik factor: Xntcorata Mindw facto r: ChrM (ogru Ma* window: ZS (OMI (tonal TZC flM d 1.*09*00. 0i*abX*4 1. 9 3.900 1.00000* M :*ntion Tin* (inet: Retenti* TLa*: RT R*C*rnc*: Tian* Window Ininal: 9**k Sl*ction: toepanae Typ : Mapena: lalynoaitl lypit f e i n t e t Oriflim f i t Vi9hting: Axis T rnuiiorM tiM : T .190. ta b tfd 0.000. Diaablto (xm l 0.390 to*v*at totaraal iaraM liai* to lu d 1/X ton* tait : 0aak*Ta-p**k a ^ lit u d a : 70 Siroot>L*g: Windev a it* (canal> Nuatar oC aootka: (Moechinv netbodi tonblad 2 1 Jo in v alley Ourasbold: Mduce p*ak ta llia O 1 Raia* baselin* t i i i w : >0.00 209.00 9.00 Dc*v v e r tic a l thr*Ael4: D*t*ct ahouldara: Shuic*r Utroahol: R attv * haighci Aao l-.ee h*ight: Rl*civ* r*a: Abao;--:* or**: 90.00 Di*aJt>l*4 30.00 1.90. ia*bld 0.00. CiaabinO 2-00. Biaablnd .0. Di**bl*4 r*s* Quattro n , 46414E SOUP 020199: FACT Equipment Log 99092 PAGE 1/1 DATE: 10-28-99 ANALYSTS STUDY NUMBER: TOXI45 MATRIX: Tween samples DESCRIPTION: dose confirmation FACT Method: Injection volume: 10 uL Cycle time: IP min. Electrode:.Z-SptK ______ Mobile Phase: (A)LP mM W 4C H3CQ2 (B)JdsQH_____________ TN-A- or stndrd number (A) 99085-11-3_______ <B)JJA222Z_ Prepared (date/by): Expires: fAl 10/21/99 mmh_______ (A) 04/00_____________ (B) la a c a g.wii 03) 2010 Store at room temp? @ or N Other:_ Guard column: None________________ Part number: na________ Lot number: na Analytical column: Keystone Betasil_________________________________ Sire: 2 x 5 0 mm_______________ Type:jClS__________ Sphere size: 5 uro Pan number 055-701-2 ________ Lot number P9E11 Serial numbcr:05918Q4Z Analytical parameters: Drying gas fL/hrl: 350 ESI nebulizing gas (L/hr) 13 LC Flow rale: 300 uL/min. Back pressure: 65 bar Sheath gas fL/hr) 0 HPLC solvent gradient: 10min-10-95 n sm VIM V IM 417.50 5LSM -S E JM . 12JL J2M 2LSL IfiJL T u n in g M ethod R e p o rt Method: C :\MXSSI/*NX\SOOTQ20199 .SRO\*COODB\BFOS3 Printed: Thu Oct 29 15:21:34 1999 Page 1 MS SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. MS Sat Rdbk 1.60 60 5 0.2 150 250 1.59 -60 -7 153 219 MSI LM Resolution HM Resolution Ion Energy Ion Energy Ramp Lens 6 Multiplier Pressures Analyser Vacuum Gas Cell Rdbk 6.le-5 4.le-3 HS2 LM Resolution HM Resolution Collision Ion Energy Ion Energy Rasp Lens 8 Lens 9 Multiplier Set Rdbk 14.0 14.0 0.9 0.0 4 650 3 Sat Rdbk 14.0 14.0 60 2.0 0.0 40 0 650 28 38 28 Method Jteport Method rii* Ue M0(Uti*di Printed: ctMcjz.Yta;\PCXJro30x9.p]to\A;Qnxviomi&-iQ-95 itearedey, October 31, 1911 l)i4 i)4 Thursday# October 31, 1999 13<44i44 Miff* 1 31100 L C Pv m v Zoic1*1 Condition* Solvents A% fi% C% D% 90.0 10.0 0.0 0.0 Flow (ml/min) Stop Tine (mins) Kin. Pressure (bar) Max Pressure (bar) Oven Temperature Left(C) Oven Temperature Right(C) 0.300 10.0 0 400 30.0 30.0 3 1 1 0 0 L C Vi i r p g r a d i e n t T l M t a l U 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 9S.0 10.0 c% 0. 0 Q.O 0. 0 0. 0 0. 0 0% 0. 0 0.0 0. 0 0. 0 0. 0 SP110Q LC Mump External I n e t Tib*table 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 Plow 0.300 0.300 0.300 0.300 0.300 Contact Off On Off Pressure 400 400 400 400 400 KP1100 JiutoiMpUr lattim i Condition Draw Speed Eject Speed (ul/min) Draw Position (mm) Scop Time (mins) Injection Volume(yl) Vial Number 200.0 200 0.00 9.00 10.0 41 MKJwd! ei\iouuinaM oiO T 30it.w \ocaam uflK C K -rvoo-saftjk~ vQ o*-s b u t M U M : m Oat IS U i i 1 1*0 rrU t* 4 > f t e Ore 3 13i44il0 it * H lv iM Delay ( bI m I t .## Sonatina t 1 M U l Mum > U f ( MS- 1 l i t e r Quutnel OeUjr < Pace i > pan 1 D*tCM 1 Scare Tine 1 Miei ) ml tl a * ( Mia* ) i Depeiti i QuuumI Iw m i DanScar ft.3 . 0.0 10. 1 Deell (Oaca) C all nervy <eV) Ceea r v i 413.00 141.0 0.3ft 30 13 v m m im i 3 a m e f 1 Haas P air f **> 1 t o u r QuuumI Delay i1 Sere ) i Spue ( Dalton* ) i Scar T1m { Mia* ) i and Tine \ nine 1 t opaata t Channel H n a t Deuphter 0.03 ft.oo 0.00 10.0 1 Buell (Sac} C ell nervy leV) Cana ( r i 1 I f f . M *1.00 0.30 3 40 Puaetioa i 3 MM m t 1 Maaa P air | * s r - ) l a t e r C h u ie ) Delay ( Saca | i Spaa < Oelteaa > < s ta r e Tlaa ( aloe ) i ad Tine { Kina 1 : Repeats i rh a w e l paraac Daubear 0.01 0.00 0.00 10.00 1 Dim11 (Sacal C ell nervy leV) 1Cana 1 v ) 1 4*1.04 11. 0.36 4S 4ft Sanction i 4 MU a< l Kara P a ir | MS- > in t e r Otanaal Delay ( Pace 1 t Spaa ( Deltona ) : S ta r t Tlaw { Kina } : ad Tine ( Kina J . Papeete Oiaeaal paraac Daughter 0.03 0.00 0.00 10.00 1 Deell (Saca) Coll aerpy (evi Cana 1 V ) 1 4 2 7 . ft. 00 0.30 40. 40 Masslynx - Sampla List Sample Usi: C:\MASSLYNX\scup020199.pro\SampleOB\102899a.SPl Printed: Thu Oc! 28 13:44:09 1999 Page 1 Page Position: (1 , i) File Name File Text MS File 1 102899001 MeOHBIk 10MIN-PFOS-POAA-PFOSA-1S 2 102899002 MeOH BIK 10MIN-PFOS-POAA-PFOSA-IS 3 102899003 FCMix-99086-431, Ippb- 9/10/99 RWW 10MIN-PFO3POAA-PFOSA-IS 4 102899004 FCMiX-99086-43-2, Sppb- 9/10/99 RWW 10MIN-PFOS-POAA-PFOSA-IS 5 102899005 FCMix-99086-43-3. lOppb- 9/10/99 RWW 10MIN-PFOS-POAA-PFOSA-IS 6 102899006 FCMix-99086-43-4, 25ppb- 9/10/99 RWW 10MIN-PFOS-POAA-PFOSA-IS 7 102899007 FCMix-99086-43-5,50ppb- 9/10/99 RWW 10MIN-PFOS-POAA-PFOSA-IS 8 102899008 FCMix-99066-43-6,100ppb- 9/10/99 RWW 1OMIN-PFOS-POAA-PFOSA-IS 9 102899009 FCMtx-99086-43-7.250ppb- 9/1099 RWW 10MIN-PFOS-POAA-PFOSA-IS 10 102B99010 FCMix-99086-43-8, SOOppb- 9/10/99 RWW 1OMIN-PFOS-POAA-PFOSA-IS 11 102899011 FCMix-99086-43-9,750ppt>- 9/10/99 RWW IQMIN-PFOS-POAArPFOSA-IS 12 102899012 MeOHBIk 10MIN-PFOS-POAA-PFOSA-IS 13 102899013 TOX145-PFOS/POAA inTwoen-dose-2ppb-1008/99 IAS 1OMIN-PFOS-POAA-PFOSA-IS 14 102899014 TOX145-PFOS/POAA InTween-ms-4ppt>-10/28/99 IAS 10MIN-PFOS-POAA-PFOSA-IS 15 102899015 FCMiX-99086-43-4,25ppb- 9/10/99 RWW 10MIN-PFOS-POAA-PFOSA-IS 16 102899016 MeOHBIk 10MIN-PFOS-POAA-PFOSA-IS 17 102899017 TOX145-PFOSAin Tween-dose-200ppb-10/28/99 IAS 10MIN-PFOS-POAA-PFOSA-IS 18 102899018 TOX145-PFOSA in Tween-ms-300ppb-1028/99 IAS 10MIN-PFOS-POAA-PFOSA-IS 19 102899019 FCMIx-99086-43-7, 250ppb- 9/10/99 RWW 10MIN-PFO3POAA-PFOSA-IS 20 102899020 MeOHBIk 10MIN-PFOS-POAA-PFOSA-IS 21 102899021 FCMix-99086-43-1, Ippb- 9/10/99 RWW 10MIN-PFOS-POAA-PFOSA-IS 22 102899022 FCMix-99086-43-2, Sppb- 9/10/99 RWW 23 102899023 FCMix-99086-43-3,10ppb- 9/10/99 RWW 10MIN-PFOS-POAA-PFOSA-IS 1OMIN-PFOS-POAA-PFOSA-IS 24 102899024 FCMix-99066-43-4,2Sppb- 9/10/99 RWW 10MIN-PFOS-POAA-PFOSA-IS 25 102899025 FCMix-99086-43-5,50ppb- 9/10/99 RWW 10MIN-PFOS-PQAA-PFOSA-IS 26 102899026 FCMix-99086-43-6, lOOppb- 9/10/99 RWW 10M1N-PFOS-POAA-PFOSA-IS 27 102899027 FCMix-99086-437, 250ppb- 9/10/99 RWW 10MIN-PFOS-POAA-PFOSA-IS 28 102899028 FCMix-99086-438. SOOppb- 9/10/99 RWW 1OMIN-PFOS-POAA-PFOSA-IS 29 102899029 FCMix-99086-439, 750ppb- 9/10/99 RWW 10MIN-PFO3POAA-PFOSA-IS CM ;r * 2> cJ o u I I I I I II i I I I I I I I I I I I I I l I ! 1 ! I I! I I I I I I I I I I I ! I I I I I ! I I'i I I ! I ! I I I I I I I I II I I I I I I I I I I I I I I I I i l I I I I I I I I I I II I I I I I I I I I I I i I l I I I I I I I OOOOOOOOOOOOOOOOOOOOOOOOOQOOO F *t- N O *> N N O CM O > O lv N n tU )(O N (O fta ff-t0 f* * S O ) * N n ^ lA (O N e O O > Q )O 9 (n Q (n < n O ttttO ln O w ( (n O i0 n O )(]iiO )O > (n n O iO iln O ) m iitiA i ~ r r r r r r T r r r r r " T"r r r r r r ; | i i S i | I . j Se I e e e e o o o o o o o q o - v r.o?ii!2!2:S?Ssg|asSS6!Sa , . <y. V. FACT: DATA REVIEW SUMMARY FORA! nU n O u i Review Sign-OIT A nalyar Review . Nunc / Otic: ~Us T v tfi: M alrix/Tim cpom u: vt<r- tu jn it Ac. <taf--t e f rff/ff SunpW L o t //Offa. Set-up A juiyru D iic/A /ulytf: In itn u n e n e "/* in (fmc/tk 0Lz*/tX T AAA a a |y t e : _______ o (OH' P Acceptable UntarRente LQ:-- iL .3 p p b __ R-2: A to m Celibntien Chockr $ - . i-2 Q j tl.r 7 ------ Extraction Blent: '/& M Matrix Blent: /< T^aa .a e * . - s ' * / --------- ~ /o * A MS/MSD: K])fr [DaUStatar fo t * ^ ____ U u d i M CCHzA n a ly te : ^ < > 5 ~PJ*~4lo*- AccAcj. ^ jA cccpU ble L in ear R an g e: fe-jojjl, -- * f r f ______________ .L O Q :. J h - 3 f> ^ L ;R,'2 : . P - n & h M a trix B la n k fr't+Jts Calibration C h e c k s X&*4. pr***- ~~2?/ '( 3 'i. MS/MSD: Data Stadie A ilytir _ S u r CcU tT>w Acceptabletineer Range: MiL O Q :_____________ ---------HkR .-2 :______________ Calibration C h e c k s tiA MS/MSD: N lfir Data Same: et-iH L n lf PAE x tra c te d B la n k M atrix B lank a /A Q u ality A n i m a t e R eview N a m e / D a te :_______________ Data Entry: _ X M f k f t f k l __ ^y . . fAH&WatrtC a e n n w n c/tJ/Juueet itrifi c a t to n i : ... (-QU. h u l.^ w k iu X t - f S f f b i P r fy p t't , * .-At?.,n d :,. Z * . j A * ' .'S i? - .. ~*- <W /-ac/- I L i ,* 'JltSC. ____ ll/fyt tx e /ic jc c f -fm kc J ls V rxf -h ________ ' J j k f * A r/f1 la v h u t/jo ,* / /v K'4S k a / . '& * j " J - M X fA c /u J tJ 4 m ~- Cftave I . c?iuf^ a / r / C &et, JfLa.'- ttAccju^ajc*,, J .L-- , >*av /^pe b o * . S)< !U c* kJ L J id e J h ' O tb d 'J i u a*aJJ< . w/f? te & jU i L J a l w t'A et h tlitr - h i o u e r l . lL'* sg j - f2 2 v ta /t - -ft ~fj~ Ja Jo .- ~~3k* Q W m jjJ S f J dL*te4L a t u * J * /a O.H C **Jr*l jUsf*L*> i^ e b*. _____________ FACT: DATA REVIEW SUMMARY FORM Dale v*hi ._ D a u Analyst: 3*5 FACT Study 4: 7 o*H"S Matrix/Timcpouits: JZj-Otr-CalJnf1 5 1<XJtf- e+J''fr> SarnptaUat: nbsn*. 1 S*tup Analysis D ate/A n aly st: In stru m en t: `' s k i L J ,-- o u m ____________________ Aaatyta: "PfbSA & Acceptablelinear Rao*e ' feZKy+L_____ LOO: R -2 . O -fH fc_________ Extrada Blank: i& S -jL tJ -t Q M a trix B lank: las-JL^-Io. CalibrationChecks OK-- fy*v~ - f " / s ~~~tr /* 'D ata Statur (X- 0 H ts re ik . fa f f V ^jiixP < P o(W . $ ) iM o T ic- D au R eview S ign-O fT A n aly il RerW w . N un / Date: 3 / * * y a f / f f Technical R rvkw N am e/D ate: O .fit.H r t o o kl / f0 Q u IU y A in in a c iiU v k w N am e/D ale: tsc tilth s D ata E a ir r 4vk t l t r pay | 1C o m m e n ts J u t U k a t l o i u : lA c < i/< v ? h i L>kJ iuJJxn-iM i rt-U 0-*d fZ- 30 rrh )O c * t * - r t- A r t b u ' - 4 L - * - fie . e d n -d to h - > ,. ,-4___ kXrt- t* cl* Ja J Srom. 4L P ert*, > 0 ) *l n f l f * IIST-STT ggS2" E' T T 777 ' lissiii s i s i s s i a s s i i s s a s s sss S * " * * " 8 8 8 8 S S 8 S 8 S S S S S S S S S E S S 3 P S a5S55 s r oos " ">3S55S SfI=sIs Sss5 =s 5 sssssrsssss jj:3MjjHK3. 2SSS88SS8 2S5g5 s f m S sSSSSiSiSH =" 8 8 8 8 8 8 " Ss3s SS ! ! is I S S3 I r * Z i c ! i i * sisasasi^ti-s-tissrs r f g g : s l ? BBfiifc f 8 1 b : i =5=E=5^SS55i===555iiisiiii^i5^^E5^Hi^53 stisiSssssgsililiisssisHsEBiiSsiSSGS ssst .3r . o . S S:S8SS3SSS*S8g8SSgSSa8Sggig* lfgggsssgggg'-sg^ligsggisgggjj = 3 3 .-s:g J 1 ! i i i c i i ! i aa Oo 99o <oI 99o 99o tyc ss| O99999909OV B |i|i||= fufinii ilfiiffi!;flffim lii*2222*222 ?cs?srtTscrsfsict ?f rers sis ill : : s m :m s s ::::::::::: 1111? !ii SiISS|SS|iS nm i Isg l a t s g Arryfs u i r r r - i S i i f i i ? ' . ! ?~?S* Vshs~ag~g* f a l l i ! V ?jf"PJpIf?S, 1' ,R -, nn r i|m|lsgs -l"" r i s s i - " ,, r. ??? g issi ? S |e| ,, fj ? n I ! "5s? c = Seee:.;. OO *999' 3M99 4999 f_ ; *S3311 3 !<f*T***T*******A-*>E*S, t *. H * * ^ * * ****** ** M UMM0909UW a * iliiii n**tn n n n > * * 0o 0o 0o 0o 0e e0o9o0o9 O -O0--9--4--0O--0-O--9-U-9- 0o 0p 0o e*. IS S oS S oS Jtig g y a w g ttw w ^ t O O Osg gW *s'9sMgMgmsi sx*g0Wg9g*s*sMsWsOs9sOss4 3 9900M0999# *OOW *a0w*sUwMxMB M<4M*MiirMiubntl W** tfUI* u* 0 * 0 0 0 0 o * O O -4O OH> M S M WU> S S * >)>'*b*xOxOxphey' My *w sm m m OX*O sss OXXO mm ooooaaaaexHxoxxcc aiSX2OMOSO5O5ooWN'pf,l-'- mmmmmm (ta S <<* X O O W M . O B f i f O a a yNM y r liH .rr|r * * p t- n S 1" f- lll O OH m r *a r 5 un S:!.U:sS s T5 tt !E gE 1 I I I SS-SS7T S' S 2 3 S S 7 -- - T 7 * e iH iiih iiu u riH iiu n m u ^ H iiih a H ii jS S g s:ss2 S 3 ssssg sss?s;g ;ssK 3 ssssg ;K s?3 s;s;s Ss -- - " - S 3 R S S 8 ^ 2 S ~ g ^ j3S 2 2 S S i |||-S S S S -S 5 S S gi3gg is S S S g S s y | I : t 1 a 3 4 OttMUfy C tU b ritiM b p a ( TO*l-rt U m . f i t y j l t e n M d m u ! '' u t . 1 1 / 4 / * m m ( (Compound 1 name: POAA (C hi) Coefficient o f 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 *# 1 ~ AnaI U 0 4 3 4 * : Q u a U t a t a d a n d t e vi f t e b y Urn w t !U1*act. U/4/MmmQuantify Calibration iiyart S S H l ' U t liv o r . bay?* doao and Compound 2 name: PFOS (Ch2) Coefficient of Determination: 0.982749 Calibration curve: 9.51640 * x + 260.801 'Response type: External Std, Area Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None hf* 2 t a a l i a PC34M: Q u a t t u u d and rovloood by ia a on U / /H Q u u a ry C alibration opar t TQX14i-n( I m r , 0y3* Ai m Mad o w i t n l ' *e. Compound 1 name: S un (Ch3) Response Factor: 4773.57 Response type: External Std, Area Curve type: RF ___ * H f* J >11 0 M 4 H : ( M M t t U M M d by U i m il/ l/ M O u w u ry CtU M aU M part TOXlli-r*C U r n . ByX* Am * bm4 > tn l- a t. IX//** IW* Compound 4 name: PFOSA (Ch4) .Coefficient o f Determination: 0.989845 jCalibration curve: 17.2655 * x + 131.101 Response type: External Std, Area jCurve type: Linear, Origin: Exclude, Weighting: 1/x, Axis nans: None A M li* Q U M tltA tM l M t W l n a d k r l M M t 1 X / I / * * i. ; Machod k|Mtc Matftod f il a : Ul bodiriad: Conpflund: P rin c M ; r : \ i M l u Mckup aap99\nnali*-r4td.pro\iathDPU10*Pv*lb Non Not M 09:20:2? 1999C l : POM. (Oill Non mov 04 Compound N>M: Incarnai M i.: OitnU ty Traa: Cm c . of standards: Oaar IF Vlua: Usar r u k fic to r : Jncagrata Window Factor: CkrMta:** u u alMta: Paak Location u ttan tlen Tina ininsl: fialati attrition Ti m : IT Mfaroftca: Tina Window la in tl : Pont Salactiwv. t JOOfIJt Maponaa Typo: Aaapoasa: CiUbdUwi C um i Polynomial Typa: Point of Origin: n t Paighcug: Aria Transformation: Concentration Unit-. Hal Pcaa-to-paak amplitude: Snootn Saoetning: Window a n a (acana) : Muabtr of laoochi: SnootMng nsthod: Baaaltnea Join allay thraahold: Reduce paak ta ilin g ; Raiae baseline nantown: Paak Separation Draw v o rtical threshold: Datact shoulder*: Shouldar threaftold: Response Threshold Mlatiw a naight; Absolute haignt: le la tiv a araa: Absoluts araa: POAA (CRD (Mono] TIC Cone, a 1.000000. Disabled i . oooeoo 2.000 1 .0 0 0 0 0 a l- * U . Enabled O.MO, OlaaPlad (Honot *.3?4 Nearest tju tn u l Araa* Uaaar Exclude in Mono SJQ Eaiblad 2 l 34.00 200.00 S.00 90.00 Disabled 30.00 1.90, 0.09. 2.00, 0.00, Disabled DlilMaO Disabled Disabled 7 i :fcoXT*a K**d 3tTp*M :*>ton*.njj <*Ta user r>i o tt - me i* * * < * --7 ? l5mmimias m*n s s -re S S* a t(T OOH? au" ! "I I OMO M UU6 S m UD* SUS S 111 1Ul s illm ffC f3t >*a sf-t H-f;l1i IS S T CSCS~ OO9 - H S 95 SS* " sc* aa *< gp ? : :Sc5 ,Iisrss, :- *1 m f<t - t arn*r E?CS*1 ( ta X i lr* Si : ? cr s S" s i r I " 1a 3 f 3 iacKsn a aCn 1" s* dis fili rfs SoSo fl t o A si *4m 4 <*m*H u a & S i; - :a- : 9 4 iii X*; : PlioOvatof;Tt*l? Xoxr Stx S S S' sfmaooa o40u "SS3 i! " 3S Il S'S Ia a ' i i* ? r g SS aeo (ic i lin 7H2 S &S *oo oMo WeO O 1 AMELIA 062498: FACT Equipment Log 99114 Quattro U, #6448E PAGE DATE: 11/05/99 ANALYST: ias STUDY NUMBER: TOX145 MATRIX: tat liver DESCRIPTION: Day 29 control and dose FACT Method: ETS-8-7.0 injection volume: 10 uL Cycle rime: 10 min. Electrode: Z-Spray Mobile Phase: (A12.0 mM NH4CH3CQ2 TN-A- or stndrd number (A) 99085-11-6 (B )McOH (B) TN-A-2997 Prepared (date/by): Expires: (A) 10/3<V99 sah (A) 04)00_____________ (B) 10/29/99 mee (B) 04/00 Store at room temp? [F] or N Other__ Guard column: None_________________ Part number: na________ Lot number na Analytical column: KcystoncBctasil_________________________________ Size: 2 x 50 mm_______________ Type: CIS__________ Sphere size: 5 urn___ Part number: 055-701-2_________ Lot number P9E11 Serial pumber089815 S Analytical parameters: Drying gas (L/hr): 300 ESI nebulizing gas (L/hr) 10 LC Flow rate: 300 ulVmin. Back pressure: 62 bar Sheath gas (L/hr)_0_ HPLC solvent gradient: lOmin-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 Tuning Method Report Method : C: \MASSLYNXVAMELIA062498.PIW\ACQCDB\PFOS1~6KV Printed: Fri Nov 05 09:43:09 1999 Paga 1 MS SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Slock Temp. Desolvation Temp. Sat Rdbk 1.60 40 5 0.2 ISO 250 1.60 -40 -3 151 253 Pressures Analyser Vacuum Gas Ce11 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 6 Lens 9 Multiplier Sat 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 10 10 I c m m iii attiad lU ip tri tktM d: U * t Hadaflad. fnt*d; C:\MkMLYMX\AHKUJUM34M. JQ\ACQt*>SUOKX*-JTOi-POfcA-tS - n t* * Han Oet 11 07:22:17 IM l rn Hav l lfl Oalvant Dalay ( aun ) : 0 .0 0 IWWH VX MM af X Maaa >ur t >- ) In ta r Chanl C;*/ i Sacs I : Span : CaUsn . S ts rt Tia : Nina Cad T iaa i Nina Sapa*tl : Channal Pat*.-.c Bauohcar l 13.JO KJ,00 0 .0 3 110.00 Owall (Saca) Coll Knajrgy <aV> 0 .3 0 30 Cona ( V 1S rwnction : 2 MRH t I taaa P a i r < l i r - | tn ta ; Tr.saral - Saca > : Sfar 1*. -r.j S t a r : r * x:r.t Cad 7 ;a . Mini 0apaa:a : Charmai Parant Dauobtar 1 4J J . 30 >0.00 00..0030 0.00 11 0 . 0 0 Dwall (Sacs) Coll tA irjy i#V| o .3 o as Cona I V <0 hM UM : 3 MM a f 1 Maaa t a l r ( I I P ' 1 Incar Channct Dali/ t Saca P : Ira n .slttn s S ta rt Tim 1;f.i End T_* Hi.-.s Sapa-, i : rr.arr. >,?** Oau^ntar 0 .0 0 0.03 0 .0 0 0.00 11 0 .0 0 Dwail fSocsi C o ll Knarqy <aV 0 .3 0 40 Co m < v ! 0 IJR C U M : 4 m m a f 1 M ua l u x ( MP> ) In ta r Cbannel Dalsy Span ! Balcons S ta r t Ti m 1 m % * . bvd. T;a I Hans 1 : ta p a i'.) : -lhar.it l ; Sacs ; D aw q h tar 0.03 0.04 0.00 10.00 ) ta I l ISac*) C oll Enarqy <aVI 4> : 7 1 .0 0 0 .4 0 COfta t V I <0 Method Report Method F ile t L ast Modified: Princad: C. \MASSZ.TXX\AKXLXA02498 .PRO\ACQUDB\l0mn-10- 95 Friday, Moveaber 05, 1599 Q6s22i24 Friday, No-rnb*r 05, 1999 09>26t29 *>ga I HP1100 LC Pump Initial Condition Solvencs A* B% C\ D% 90.0 10.0 0.0 0.0 Flow (ral/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 6.00 A% 90.0 90.0 5.0 5.0 90.0 B% 10.0 10.0 95.0 95.0 10.0 c% 0.0 0.0 0.0 0.0 0.0 D% 0.0 0.0 0.0 0.0 0.0 Flow 0.300 0.300 0.300 0.300 0.300 Pressure 400 400 400 400 40C HP1100 LC Pump External Event Ti.table 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 Autosajsplar 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 32 Massiynx - SampJ List Sample Ust: C:\MASSLYNX\amelia062498.PROVSampleDBVt1G599a.SPl Printed: Fri Nov OS09:25:34 1999 Page Positior File Name File Text MS File 1 110599001 MeOH Blank lOMIN-PFOS-POAA-IS-PFOSA 2 110599002 MeOH Blank 10MIN-PFOS-POAA-IS-PFOSA 3 110599003 MeOH Blank 10MIN-PFOS-POAA-IS-PFOSA 4 110599004 TOX145-RBL11049WBIk-1, RWW-Box 99-211 lOMIN-PFOS-POAA-IS-PFOSA 5 110599005 TOX145-RBL11049RBLBIk-1, RWW-Box 99211 10MIN-PFOS-POAA-IS-PFOSA 6 110599006 TOX145-RBL110496ppb-1. RWW-Box 99211 lOMIN-PFOS-POAA-IS-PFOSA 7 110599007 TOX145-RBL1104912ppt>-1, RWW-Box 99211 lOMIN-PFOS-POAA-IS-PFOSA 8 110599008 TOX145-RBL1104930ppt>-1. RWW- Box 99211 lOMIN-PFOS-POAA-IS-PFOSA 9 110599009 TOX145-RBL1104960ppt>-1, RWW-Box 99211 10MIN-PFOS-POAA-IS-PFOSA 10 110599010 TOX145-RBLl1049120ppt>-1, RWW-Box 99211 lOMIN-PFOS-POAA-IS-PFOSA 1 1 110599011 TQX145-RBL11049300ppt>-1, RWW-Box 89211 10M1N-PFOS-PQAA-IS-PFOSA 12 110599012 TOX145-RBL11049600ppb-1, RWW- Box 99211 lOMIN-PFOS-POAA-IS-PFOSA 13 110599013 TOX145-RBL1l049900ppl>-1, RWW- Box 99211 lOMIN-PFOS-POAA-IS-PFOSA 14 110599014 TQX145-RBL110491200ppb-1, RWW-Box 99211 lOMIN-PFOS-POAA-IS-PFOSA 15 110599015 MeOH Blank lOMIN-PFOS-POAA-IS-PFOSA 1 6 110599016 TOX145-RBL, 9R03249300pp9MS, 11/4799 Box 99211 lOMIN-PFOS-POAA-IS-PFOSA 17 110599017 TOX145-RBL. 9R03240-300pp9MSO. 11/4/99 Box 99211 lOMIN-PFOS-POAA-IS-PFOSA 18 110599018 TOX145-RBL 9R03240/M/Day29/Contnol, 11/4/99 10MIN-PFOS-POAA-IS-PFOSA 19 110599019 TOX149RBL. 9R03241/M/Oay29/ConirDl, 11/4/99 lOMIN-PFOS-POAA-IS-PFOSA 20 110599020 TOX145-RBL. 9R03242/M/Day29/Control, 11/4/99 lOMIN-PFOS-POAA-IS-PFOSA 21 110599021 TOX145-RBL11049-300ppb-CC1-1. RWW-Box 99211 10MIN-PFOS-POAA-IS-PFOSA 22 110599022 MeOH Blank lOMIN-PFOS-POAA-IS-PFOSA 23 110599023 TQX145-RBL, 9R03243/M/Day29/Control, 11/4/99 lOMIN-PFOS-POAA-IS-PFOSA 24 110599024 TOX145-RBL, 9R03244/M/Day29/Contti>l, 11/4/99 lOMIN-PFOS-POAA-IS-PFOSA 25 110599025 TOX145-RBL, 9R03255/M/Day29/5m(j/kg. 11/4/99 lOMIN-PFOS-POAA-IS-PFOSA 26 110599026 TOX145-RBL. 9R03256/M/Day29/5mo/kO. 11/4/99 lOMIN-PFOS-POAA-IS-PFOSA 27 110599027 TOX145-RBL. 9R03257/M/Day29/5mg/kg. 11/4/99 lOMIN-PFOS-POAA-IS-PFOSA 2S 110599028 T0X145-RBL11049-300ppb-CC1-2, RWW- Box 99211 lOMIN-PFOS-POAA-IS-PFOSA 29 110599029 MeOH Blank lOMIN-PFOS-POAA-IS-PFOSA 30 110599030 T0X145-RBL, 9R03258/M/Day29/5mgrttg, 11/4/99 lOMIN-PFOS-POAA-IS-PFOSA 31 110599031 TOX145-RBL. 9R032S9/M/Day29/5mg/kg. 11/4/99 lOMIN-PFOS-POAA-IS-PFOSA 32 110599032 TOX145-RBL11049-300ppi>-CC1-1. RWW- Box 99211 lOMIN-PFOS-POAA-IS-PFOSA 33 110599033 MeOH Blank lOMIN-PFOS-POAA-IS-PFOSA 34 110599034 TOX145-RBL11049-WBIk-1, RWW- Bax99211 lOMIN-PFOS-POAA-IS-PFOSA 35 110599035 TOX145-RBL11049-RBLBIk-1, RWW- Box 99211 lOMIN-PFOS-POAA-IS-PFOSA 36 110599036 TOX145-RBL11049-6ppb-1. RWW-BOX 99211 10MIN-PFOS-POAA4S-PFQSA 37 .110599037 TOX14S-RBL11049-12ppb-1. RWW- Box 99211 lO M IN -P F O S -P O A A -IS -P F O S A 38 110599038 TOX145-RBL11049-30ppt>-1. RWW- Box 99211 lOMIN-PFOS-POAA-IS-PFOSA 39 110599039 TOX145-RBL11O49-0ppb-1. RWW- Box 99211 IQMiN-PFOS-POAA-tS-PFOSA 40 110599040 TOX145-RBL11049-120ppO-1.RWW-Box99-211 lOMIN-PFOS-POAA-IS-PFOSA 41 110599041 TOX145-RBL11049-300ppt>-1. RWW-Box 99211 lOMIN-PFOS-POAA-IS-PFOSA 42 110599042 TOX145-RBL11049-600ppt>-1. RWW-Box99211 lOMIN-PFOS-POAA-IS-PFOSA 43 110599043 TOX145-RBL11049-900ppt>-1. RWW-Box 99-211 10MIN-PFOS-POAA-IS-PFOSA 44 110599044 TOX145-RBL11049-1200ppb-1, RWW-Box 99211 lOMIN-PFOS-POAA-IS-PFOSA i M asslynx - S am p le Llat Sample List: C:tMASSLYNX'amelia062498.PRO\SampleOB\110599a.SPL Primed: Fri Nov 05 09:25:34 1999 kO(eo>soi(flbUK)->o<0s>so)uijwN>iopaNOM/iMdMue S S 5- a < ooooooooooooooooooooooooooaoooooooaooQOooooo I I I i 11111111111111111111 So' I I I I ! I I I I I I I I I I II I M I I I I I I! I I t I I 1I I I I I I I I I I I I I I !l I I I I I I I I I I I II I I I I I I I I I I ! I I I I I I I I II 1 I I g> S > ooa 9 I I I II I I I I I I I I I I I I i I I I I I I I I I I I I I I I I I I I I I I I I N | o o sI ! I I i I I i I i I I 1 M I H I I ! I i I I I I I I I I I I I I ! I I I I I I I I go o I I ! I I I I i I I U I ! ! U I l I I i I I I I I i I I I I I 1 i 1 1 S ! i M 1 1 a?o m ! ! ! ! ! S ! ! i II I i ! i ! ! ! 1 ! ! ! ! } ! i I ! ! I I ! i } ! ! I ! I ! ! f ! I ^ a 9 2 Page Positior.. (2.1) FACT: DATA REVIEW SUMMARY FORM Dale `j u hn D *u A nalyst FACT Study I: JkM - Mstrix/Tinicpoints: LU *f 2 j ie - g g / tf/# SvnpU U at -Jt/offA _______________________ Sel-up Analysis D*te/A nalyst instrument J S i X " i/d n &O>dU~^r o z / t L . ( V7AAA n aly te: ^,/u : / jAcceptable LinearRange: t& t& h - jm ^ L LOO /Z tTffl------------ ;Ra2: 0-V O tSL Extraction B lack: _ MMn* Binde /fS -/L * . Coo. KC alibration C b e c k x Z t L M S/M S D :____ D f l l r , n o i - \ i u A ' J ^ a .\c ,rtf} Dili Sana: fofllj IA n aly te: 7fcs Cfvnc i, *) jA cceptable L in a r Range: i fLoo-. n & p p L R-2: . .W /Y Z ? ft-P^L. --------* t t t t j r l Extracted BUnlc W M Matrix BUnlc^ r e iJ c ih u ^ t0 0 OK(calib ratio n C h eek s: - / ? '/ ____________________ MS/MSD:---M Onnlyii. Isi.'U -IW-_. D ata Statue oie g o W u t, nfirhi CFuu.cJ ' ) Acceptable L i n a r R ange. V -LOQ-. 1 R'2. Q.fM3f /3J pr>C fa titi E x tracted B U nlc Jtsms J L sJ qsl M atrix B U nlc Jrss 41ak CQ Ok-C alibration C hecks: - z & ______________ MS,MSD:-- Oa^-Q m>l m a rl r tr tA fco, Onl^r.r DauSatus: Q,, I t lo s M lA f. IlltShS D a ta R ev iew S ip t-O fT Analyst Review H em e IOtic. 3 S ' I h i Teehokal Review N am e/D ate: Tnee fniM f ^ liov-IS-ft Quality Aaauraaca RavUw N a m e/D ate:____________ Data Entry:. LAC Comments / JufttUlcatfams: * 111 l u I d f J' Spumi'fa-/ hs , , ( l -pjttrt f e . 3o. / lf-3y*L ),__________ h jL ir H u h __- f i t *jctfa.ci/iK . U m '} ___ +H .j& u d s P ert w in d e d J x e -a ,_____ -U O ust*. 1i J iS u S - h i^ ____J_a__Je__-_____ t o y 4 lu d x a tj L t t X i c e n ----------- S iW ifim - lL a e d c tf y L cJ' LcSiLt f r ^ j t s L-J. Xf / t < J - / L .gOjuMaiL l- k - T h s 'M <9L/o. ut Curt*cypas i d . i .rfrpL W e ld e d a s i j m . J i s l j > S n . sd 4*- d k CUrtKS. ItJtK ffhig J a a ltd Qix r a ,, n t K . m &L j& tr w td c .4 ? fiftw/rttuf fp(T) : POAA \M (urf- o-__ S /L rtflc J t j * MVW* -*1 2 FACT: DATA REVIEW SUMMARY FORM Dale: D a u AnaJyit: M:F A C T Study Jus Murix/Tiraepotnts: r-- i r r r y --21. <fe$< SAITtpl L ift /f/OffA <*/ Yf/ff S et-up Analysis Datc/A nalysc lA i "//-h i Instrum ent f A n a ly te :___ QUfr ( F ^ </_f_____________________ f/AA cceataM e L in e a r R in u s : LOQ: HA FE x tra c tio n B lan k : a R ^: AM M atrix B lank M ____________ C alibation Checks: A fc M S/M SD: M o^C. 4 a ro J- D ate Statue P n rJn k -, D a U iT rio i used- ^ ^thrift D ili Review Sign-OIT A nalyst Review Name /D a le T echnical R avkw tiXtrN am / D ele: t o J>c.y. lo V J- iXC Q vtlltjr A a u n s c a R rvtew N a m e / D a t e : _______ ________ Data B atty: _ UC. lih rh l Com nM Qts / Ju stin c a tio a s: X J c r u J < [J levels Juctrc J a u /- "A * J i /u -J ra h tS i'g 7ju.____ JtfuJto. / t d e y - o ~ - ~JL S ju k e J ? I I "gassa-- : i ssssssssssa J " "U nni ! iissiiiiii I =S=5S=35?S5 a ||SSTSTT s sssgssssass 5 ' "" 2 5 5 t iiii 5 ssasssss 1200pvb-2, I i' s - . - 7 ? . T ^ S-'-a-r*'! * " *sfas*sssiaat?ss3ssss 1............. 3 a s 5 S S 2 * s s S s S s " * " -- I s S S ilililsiiialiilliaiii i= --3 5 S S 5 5 s|5 |S |g 5 g f|= S 5 S 5 2 S g | i -lliillil 'i 3*S3S*S=SSSSS2SSS5 S3333a3SSS5SqSSSRS5SSS3 Va i 3 t i I ! ! 3 1 On i |S R 5S |g ||]!i!j|a||g | liliiiiU llllllilH IS llim illiH I |558SS 8 S 3 ||" " |s g 5 S 5 I3 || i55iS55H5SS5552S5S55S255SS s lilIlills S -Iissste llI S sIIIIS ssrrrrsssisissssssrssisis ,, u. . s w: : s s s I >, ; s f f Ornaci (y u l l k r i U tapare ____ TOU3rac U v w , le y I mm llMXaaa- M t. 11/1/* W >a I 3019*1 f t t u t lU I ! * r iM d fey la # * 1 1/11/99 n u n - r * t i i w , n r a t m A i u * m - .. U / l / H au I l M l l i gw--l i t e t t e tinte kr tu Mii/u/ii OMM ltr OXlkrMlM u r n TOXH(S-rc U r n , t e r tea* U n l w > t m . 11//## * 3 M i m i) i fltMMlte* atei pftat4 hr l u m U /U /ll w M lty GallkrMtM l a p m lQ U IS < n t U m , 4y a t 4m U t t l m - m . 1 1 /4 ! m m IMUtl Om k IU M Mi prtMt hjr U i m U/U/H HH HO*I*D*H**H :::: ssr ? ooo O HH m El il i l" n ! I ti li ! n \ I HH ss far * a a e oo u apo till Si s i*! fil HH fl se iti i il tflr. * || Pi I fis f? rs| :1s I i jf rt f !f I - ?- t i f I fis " f i fl 1 * w i s si 1 i? lu -iPo* ! Il lisi . 1. oo IpO as 1= n 1: Ii u i 3s i! i aa :] s im o: 2 _ tU lili liliU"6u ilii! iMph<jl i> |iJ Jv 221 3 i Ili ;Ilji .il J>J;V>! 3. I a S sj ssa!>i.:.a.;3:Ja !il ? i !f s: m a i, . V*r im m ft O M fMt H i) i|i n Quattro II, #<414E SOUP 020199: FACT Equipment Log 99092 PAGE 1/1 DATE: 11:10-99 ANALYSTijaj STUDY NUMBER:TOXI45 MATRIX: rat liver DESCRIPTION: djlmigns-dayW FACT Method: ETS-8-7.0 Injection volume: 10 uL Cycle time: 10 min. Electrode:iSB3X______ MobUe Phase: fA12.0 mM NH4CH3C02 (BXMsQH------------------- TN-A- or stndrd number (A) 99085-11-21_______ (B).JT7-A-338ti________ Prepared (date/by): IA111/6/99 sah_______ (B) H/$/9gjah-- Expires: (A) 04/00_____________ (B)_201fi_____________ Store at room temp? @ or N Other:_____________________ _ Guard column: None________________ Pan number: na________ Lot number:jja______________________ Analytical column: Keystone Betasil_______________________________ _ Size: 2 x 50 mm______________ Type:jQ18__________ Sphere size:JLaB___________ Pan number: 055-701-2_________ Lot number: P9E11 Serial number:Q591804Z______ Analytical parameters: Drying gas fL/hrl: 350 ESI nebulizing gas (L/hr) 13 LC Flow rate: 300 uL/min. Back pressure: 65 bar Sheath gas (L/hr)JJ____ HPLC solvent gradient: 10min-I0-95 Time (min.! no.oo 2) 1.00 3) 3 .3 0 4) 7.50 5I52Q __________ .,M _ _1M 1M _ .2 1 2 . 252122_ Tuning Method Report Method: C: \MASSL-nmSOTP020199-PROVACQUDB\PrOS3 Printed: Nad Nov 10 10:49s41 1999 Page i MS SOURCE ( ESP- ) Capillary Cone Extractor RF Lens Source Block Temp. Desolvation Temp. M52 s*t' RdMc 1.60 40 5 0.2 150 250 1.61 -60 -6 150 250 Pressures Analyser Vacuum Gas Cell Kdbk 6.Qe-5 4.le-3 MSI LM Resolution KM 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 Sat 14.0 14.0 0.9 0.0 4 650 Sat 14.0 14.0 10 2.0 0.0 40 0 650 Method jUkport Method Fil: Let Modified: WCet d\nMeMe*dLaIyMXVfMOgC9f0b3t01r991.0PI1O9\9A9CQ1a0i*I1*3\11007min-10-93 Wednesday, HotMbir 10 1999 10*49*30 rtf i 91100 LC rap Zaltitl condition* Solvents A% fi% C% D% 90.0 10.0 0 .0 0 .0 Flow (ml/min) Scop Time (mins) Min Pressure (bar) Max Pressure (bar) Oven Teznperacure l#eft(C) Oven Temperature Right(C) 0.300 10.0 0 400 30.0 30.0 91100 LC Sump Sradien* Timetable The gradient Timetable contains 5 entries which are : Time A% fi% 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 Pressure 400 400 400 400 400 91100 LC Pump external Knot 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 91100 Aucoiueltr Initial emulitione Draw Speed Eject Speed (ul/min) Draw Position (inn) Stop Time (mins) Injection Volume(pi) Vial Number 200.0 200 0.00 9.00 10.0 91 Maaslynx - Sample Usi Sample Ust: C:\MASSLYNX\soup020199.pro\SampleDSVI11099a.SPL Printed: Wed Nov 1010:48:56 1999 Page 1 Page Position: (1,1) Rie Name Rie Text MS Rie 1 111099001 MeOHBlank 10MIN-PFOS-POAA-PFOSA-IS 2 111099002 MeOH Blank 1OMIN-PFOS-POAA-PFOSA-IS 3 111099003 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 4 111099004 TOX145-RBL11049-WBIk-2. RWW 1OMIN-PFOS-POAA-PFOSA-IS 5 111099005 TOX145-RBl.11049-RBlBlk-2.RWW 1OMIN-PFOS-POAA-PFOSA-IS 6 111099006 TOX145-R8L11Q49-6PP-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 7 111099007 TOX145-R8l.11049-12ppb-2.RWW 10MIN-PFOS-POAA-PFOSA-IS 8 111099008 TOX145*RBL11049-3Qppb-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 9 111099009 TOX145-RBL11049-60ppb-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 10 111099010 TOX145-RBL11049-120ppb-Z RWW 10MIN-PFOS-POAA-PFOSA-IS 11 111099011 TOX145-RBL11049-300ppb-2. RWW 10MIN-PFOS-POAA-PFOSA-IS 12 111099012 TOX145-RBL11049-800ppb-2. RWW 10MIN-PFOS-POAA-PFOSA-IS 13 111099013 TOX145-HBL11049-900ppb-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 14 111099014 TOX145-RBL11049-1200ppb-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 15 111099015 MeOH Blank 10MIN-PFQS-POAA-PFOSA-IS 16 111099016 TOX145-RTL, 9B03255/M/Day29/5mg/kg-0100.11/4/99 10MIN-PFOS-POAA-PFOSA-IS 17 111099017 TOX145-RTL.9R0325fl/M/Day29/5mQ/kg-D100,11/49 10MIN-PFOS-POAA-PFOSA-IS 18 111099018 TOX145-RTL, 9R03257/M/Day29mg/Vfl-D100,11/4/99 10MIN-PFOS-POAA-PFOSA-IS 19 111099019 TOX145-RTU 9RO325a/M/Day2a/5m9'kg-01OO,11/4/99 10MIN-PFOS-POAA-PFOSA-IS 2 0 111099020 TOX145-RTL9R03259/M/Day29/5mofk9-D100,11/4/99 10MIN-PFOS-POAA-PFOSA-IS 21 111099021 TOX145-RBL11049-300PP6-CC1-2.RWW 10MIN-PFOS-POAA-PFOSA-IS 22 111099022 MeOH Blank 10MIN-PFOS-POAA-PFOSA-IS 23 111099023 TOX145-RBL11049-WBIk-2. RWW 10MIN-PFOS-POAA-PFOSA-IS 24 111099024 TOX145-RBL11049-RBlBlk-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 25 111099025 TOX145-RBL11049-6ppb-2, RWW 10MIN-PFOS-POAA-PFOSA-1S 26 111099026 TOX14S-RBL11049-12ppb-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 27 111099027 TOX145-RBL11049-30PP-2. RWW 10MIN-PFOS-POAA-PFOSA-IS 28 111099028 TOXI45-R8L11049-60ppb-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 29 111099029 TOX145-RBL11049*120ppb-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 30 111099030 TOX145-RBL11049-300ppb-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 31 111099031 TOX145-R8L11049-600ppb-2,RWW 10MIN-PFOS-POAA-PFOSA-IS 32 111099032 TOX145-R8L11049-900ppb-2. RWW 10MIN-PFOS-POAA-PFOSA-IS 33 111099033 TOX145-RBL11049-1200ppb-2, RWW 10MIN-PFOS-POAA-PFOSA-IS 34 111099034 TOX145-R8L11049-9C0ppb-2, RWW 10MIN-PFOS-POAA-PFOSA-IS Masstynx - Sim pl List , Sample List: C:\MASSLYNX\soup020199.pro\SampleD8\111099a.SPL Printe* Wed Nov 10 10:48:56 1999 Inlet File Bottie Inject Volume Sample Type Conc A Conc B C o r te C 1 10min-10-95 91 2 10min-10-95 91 3 10min-10-95 91 4 10min-10-95 1 5 10min-10-95 2 6 10min-10-95 3 7 10min-10-95 4 8 10min-10-95 5 9 10min-10-95 6 10 10min-10-95 7 11 10min-10-95 8 12 10min-10-95 9 13 10mirv-10-95 10 14 10mitv 10-95 11 15 10min-10-95 92 16 10mln-10-95 12 17 10min-10-95 13 18 10min-10-95 14 19 10min-10-95 15 20 10min-10-95 16 21 10min-10-95 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 2 t 10rron~10-95 6 29 10min-10-95 7 30 10min-10*95 8 31 10min-10-95 9 32 10min-1O-95 10 33 10min-10-95 11 34 10min-10-95 12 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- IQ -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- io -- 10 -- 10 -- 10 -- 10 -- 10 -- 10 -- Pago 2 Pago Position: (2,1)