Document B5Q7ooRgwa4DJNO2p78j6brDk

/H U i -03r? ACUTE TOXICITY TO AQUATIC INVERTABRATES (DAPHNIA MAGNA) TEST SUBSTANCE Identity: Perfluorooctanesulfonylamido(ethyl)acetate; may also be referred to as PFOSAA, FC-128 or as the major component of FC-127, FC-129, FC-109, or FC-109-X. (Glycine, N-ethyl-N[(heptadecafluorooctyl)sulfonyl]-, potassium salt, CAS # 299151-7) Rem arks: The test sample is FC -109-X referred to by the test laboratory as E2566-2. Current information indicates it is a mixture of 1923% test substance, 61% water, 12% 2-methoxymethylethoxypropanol, 2% ethanol, and 2-6% C4-C7 fluoroalkyl carboxylate compounds. Test sample was from 3M production lot 2. The following summary is abbreviated because the test sample is a mixture of the test substance in a water/organic solvent solution. Data may not accurately relate toxicity of the test sample with that of the test substance. METHOD: Methods: OECD 202 Test type: Static acute GLP: Yes Year Completed: 1988 Species: Daphnia magna Analytical monitoring: Temperature, pH, and DO RESULTS Nom inal concentrations: Bk control, 1 .0 ,1 .8 , 3.2, 5 .6 ,1 0 ,1 8 , 32 mg/L Elem ent values: 24-hour LC50 = >32 mg/L (estimated) 24-hour NOEL = 32 mg/L 48-hour LC50 = 1.5 (1.0-1.8) mg/L 48-hour NOEL = 1.0 mg/L All element values based on nominal concentrations. Rem arks: Testing was conducted on the mixture of the test substance as described in the test substance remarks field. The value reported applies to that mixture and not the test substance. No attempt was made to determine the impact of the presence of the organic solvents or what portion of the toxicity can be contributed to the Perfluorooctanesulfonylamido(ethyl)acetate. 00Q 255 CONCLUSIONS The FC-109-X 48-hour LC50 for Daphnia magna was determined to be 1.5 mg/L with a 95% confidence interval of 1.0-1.8 mg/L. The 48-hour no observed effect level was 1.0 mg/L. Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 DATA QUALITY Reliability: Klimisch ranking 2. Testing meets all criteria for quality testing, but lacks analytical confirmation of test substance concentrations. There is a lack of characterization of the test sample. REFERENCES This study was conducted at Analytical Bio-Chemistry Laboratories, Inc. of Columbia, Missouri at the request of the 3M Company. OTHER Last changed: 5/18/00 000256 SPONSOR 3M Company Attn: Mr. Mohamed Elnabaravy EE & PC Environmental Labs Building 21-2V-05, 900 Bush Avenue St. Paul, Minnesota 55106 STUDY TITLE Acute Toxicity of E2566-2 to Daphnia magna DATA REQUIREMENT OECD Guideline 202 AUTHOR Scott Frazier Biologist II STUDY COMPLETED ON January 9, 1988 PERFORMING LABORATORY Analytical Bio-Chemistry Laboratories, Inc. Aquatic Toxicology Division 7200 East ABC Lane P.O. Box 1097 Columbia, Missouri 65205 ABC LABORATORY PROJECT ID #36616 Pa^_ l ot **8 0 0 0 2 5 BEST COPY AVAILABLE Submitted By: Analytical Bio-Chemistry Laboratories, Inc. 72C0 East ABC Lane P. 0. Box 1097 Columbia, Missouri 65205 (314) 474-8579 Prepared By: fl'l ;/ /> l( i :L J / ' M 'a Michael Ruddy Biological Technician 11 Scott Frazier ' -- ^ Biologist II/Study Director Date //(5 } Date Approved By: M rAlan D. Forbis Supervisor, Invertebrate/ Bioconcentration Investigations Date :dab23 Kathy LAndholt Quality Assurance Officer / > '/ ? i " ..... .... Carl M. Thompson Aquatic Toxicology Manager iiiih ? `D a t e f--i -V*' Date 0 o -r>3 r; s ABC LABS #36616-2 of 48 BESTCOPY AVAILABLE TABLE OF CONTENTS Page No . LIST OF TABLES...................................................... 36616-4 PROJECT PERSONNEL .................................................. 36616-5 INVERTEBRATE ACUTE TOXICITY COMPENDIUM........................... 36616-6 S U M M A R Y .................................. .......................... 36616-7 INTRODUCTION......................................................... 36616-8 METHODS AND MATERIALS ............................................. 36616-8 I. Test Organises........................................... 36616-S II. Test Procedure............................................ 36616-8 III. Test C o m p o u n d ............................................ 36616-9 IV. Statistics.............................. 36616-9 R E S U L T S .................................. .. . . . ................ 36616-9 LITERATURE CITED............................. ................. 36616-13 QUALITY ASSURANCE STATEMENT ......... * * * ...................... 36616-14 STUDY COMPLIANCE STATEMENT........... ............................. 36616-15 APPENDIX - RAW DATA ................ . . . . . . . . . . . . . . 36616-16 re* ABC LABS 036616-3 of 48 BEST COPY AVAILABLE Table No. 1 2 3 LIST OF TABLES Page No. Chemical Characteristics of Well Water Used by ABC's Aquatic Toxicology Division................ 36616-10 Acute Toxicity of E2566-2 to Daphnia x a g n a ......... 36616-11 Percent Mortality and Water Quality Measurements During the Acute Toxicity Test of E2566-2 to Daphnia magna ......................... 36616-12 0 o (*2G o ABC LABS #36616-4 of 48 BEST COPY AVAILABLE PROJECT PERSONNEL The Study Director of the project for Analytical Bic-Checistry Laboratories, Inc. was Scott Frazier, Biologist II. Supervising the conduct of the study for 3M Company was Mr. Kohamed Elnabarawy. The followin'; ABC personnel assisted with various phases of the study. Name Michael Ruddy Scott Frazier Jeffrey Latham Title Biological Technician II Biologist II Biological Technician I Initials i: j t-- 000201 ABC LABS 36616-5 of 48 BEST COPY AVAILABLE INVERTEBRATE ACUTE TOXICITY COMPENDIUM Subject: "Acute Toxicity of E2566-2 to Daphnia magna." ABC Study Number 36616. Sponsor: 3M Company Testing Facility: Analytical Bio-Chemistry Laboratories, Inc. Aquatic Toxicology Division P.O. Box 1097 Columbia, Missouri 65205 (314-474-65.'9} Location of Original Raw Data and Final Report: 3M Company EE & PC Environmental Labs Building 21-2V-05, 900 3ush Avenue St. Paul, Minnesota Test Material: E2566-2 Test Concentrations: Control, 1.0, 1.8, 3.2, 5.6, 10, 18 and 32 mg/1. Dilution Water: 246 mg/1 (hardness), 178 mg/1 (alkalinity), 8.0 (pH). Test Dates: Initiation - January 7, 1988 Termination - January 9, 1988 Length of Study: 48 hours Results: 24-hour LC^q * >32 mg/1 (estimated) 24-hour NOEL - 32 mg/1 48-hour LC50 * 1.5 mg/1 (952 C.I. - 1.0-1.8 mg/1) 48-hour NOEL " 1.0 mg/1 Test Species: Daphnia magna Source of Organisms: ABC Laboratories in-house culture. Age of Organisms at Study Initiation: First-instar (<J4 hours old) 00026.2.- ABC J.ABS #36616-6 of 48 BEST COPY AVAILABLE SUMMARY The acute toxicity of E2566-2 to Daphnia magna was assessed using the methods outlined by the Committee on Methods fot Toxicity Tests with Aquatic Organisms. Water quality parameters of temperature, dissolved oxygen and pH were measured at the termination of the test and were within acceptable limits. The results of the 48-hour static Daphnia magna toxicity study are summarized below. All reported values were based upon nominal concen trations. Compound 2566-1 24-Hour LC 50 >32 mg/1 (estimated) 48-Hour LC 50 (95'C.I.) (1.0-1.8 mg/1) The 14 and 48 hour no-effect levels of E2566-2 based on the absence of mortality and abnormal effects were 32 and 1.0 tng/1, respectively. ABC LABS #36616-7 of 48 BEST COPY AVAILABLE INTRODUCTION This definitive static bioassay was performed by the Aquatic Toxicology Division of Analytical Bio-Chemistry Laboratories, Inc., Columbia, Missouri, for 3M Company, from January 7, 1988 to January 9, 1988. The purpose of this test was to determine the 24- and 48-hour LC.q levels for E2566-2 to Daphnla magna. The study was performed using ABC Protocol 07806 as approved by Mr. Mohamed Elnabaravy, 3M Company, on January 7, 1988. METHODS AND MATERIALS The procedures for static bioassay, aa described in Methods of Acute Toxlcltv Tests with Fish. Macroinvertebrates and Amphibians (.I) and Standard Methods for Examination of Water and Wastewater (2), were used In this experiment. 1. Test Organisms The Daphnla magna used in the test were cultured at the A3C facilities in well water (Table 1). The adult daphnlds were fed algae (Selenastrum capricornutnm) at least every three days prior to testing and supplemented with a suspension of Tetraisin, cereal leaves, vitamin solution and yeast. The daphnids were identified to species using the taxonomic key presented by Pcnnak (3). II. Test Procedure The static Daphnla bloassay was conducted in 250-ml glass beakers containing 200 ml of daphnid culture/test water. All test vessels were covered with loose-fitting petrl dish covers to minimize evaporation and protect, against contamination during the study. These vessels were kept at 20 (12.0) C in a temperature controlled area. The lighting was maintained at 50-70 footcandles on a 16-hour daylight photoperiod with 30-minute simulated dawn and dusk periods. An initial range-finding experiment was conducted using ten Daphnla each in exposure concentrations of 1.0, 10, and 100 mg/1. From these results, seven treatment concentrations in duplicate with ten Daphnla (first instar less than 24 hours old) per beaker were selected for the definitive bioassay. These concentrations were a logarithmic series ranging from ... I . ? to 32 mg/1 and included a control. Ail concentrations were observed once every 24 hours for mortality and abnormal effects such as surfacing, clumping of the daphnlds together and daphnids tending to the bottom of test chambers. Water chemistry parameters of temperature, dissolved oxygen and pH were measured in the control, low, middle and high concen trations at 0 and 48 hours. - ABC LABS 036616-8 of 48 BEST copy AVAILABLE III. IV. Test Compound The F2566-2 sample was received on December 29, 1987 as a loamy, yellow liquid and was stored at room temperature in darkness. Sample purity was unspecified. Test concentrations were prepared based on total product. All standard weights and dilutions can be found in the Appendix. Daphu^d culture/test water was used in the preparation of all working stock solutions. Statistics Statistical analysis of the concentration vs. effect data (generally mortality) was obtained by employing a computerized LCCq program developed by Stephan et al. (4). This program calculated the LC,.q statistic and its 95 percent confidence H a l t s using the Binomial, the moving average and the probit tests. Three different methods of analyzing the data were used since no one method of analysis is appropriate for all possible sets of data that may be obtained. The method of calculation selected for presentation in this report was that which gave the narrowest confidence limits for the LC,.q (4, 5) although all three models are valid. However, if no mortality occurred or if a dose response could not be demonstrated over a reasonable range (<37 to >63Z) an LC.q and/or its 95 percent confidence limits could not be calculated. RESULTS Table 2 presents the estimated and calculated LC,_ values and 95-percent confidence intervals for E2566-2. The 24- ana 48-hour LC,.. values were >32 (estimated) and 1.5 mg/1, respectively. All results were based on the nominal concentrations of 1.0, 1.8, 3.2, 5.6, 10, 18 and 32 mg/1. The no-effect concentration based on the absence of mortality and abnormal effects was 32 mg/1 at 24 hours. At 48 hours the no-effect level was 1.0 mg/I. The abnormal effect of mortality was observed In the 1.8, 3.2, 5.6, 10, 18 and 32 mg/1 test concentrations. The 10, 18 and 32 mg/1 test concentrations were observed at 24 and 48 hours to have a surface film and precipitate present. Table 3 presents the percent mortality and water quality parameters measured during the test. The dissolved oxygen concentrations ranged between 8.7 and 9.5 mg/1. These values represented 100 and 107-percent saturation at 20 and 19 C (corrected for local altitudinal pressure), .^respectively, and were considered adequate for testing (1). The pH values of the test solutions ranged from 8.2 to 3.4 and were consistent with the .. 'ntrol. The study was conducted following the intent of the Good Laboratory Practice Regulations (6) and the final report was reviewed b y Analytical Bic-Cfcesistry Laboratories' Quality Assurance Unit. All original raw data were provided to 3M Company, with a copy retained at Analytical Bio-Chemistry Laboratories, 000205., ABC LABS d36616-9 of 48 BEST COPY AVAILABLE TABLE l Chemical Characteristics of Well Water Used by ABC's Aquatic Toxicology Division. Parameter Temperature Dissolved Oxygena pH Hardness (CaCO-j) Alkalinity (CaC03) Conductivity Total Organic Carbon Suspended Solids Aluminum Arsenic Boron Cadmium Chromium Cobalt Copper Iron Lead Mercury Nickel Silver Zinc Measured organophosphorus pesticides Measured organochlorine pesticides plus PCB's Concentration 17 - 22*Cb 7,4 - 9.1 ppmb 7.6 - 8.4b 206 - 275 ppmb 224 - 336 ppmb 500 - 650 umhos/cmb 1.4 ppmC (0.9 - 2.8 ppm)*^ 0 - 1 . 3 ppmb <10 ppb < 1 ppb 2.25 ppm <3 ppb <7 ppb <3 ppb <3 ppb 14 ppb <30 ppb 0.43 ppb <8 ppb <4 ppb 2 ppb <0.14 ppb <1.0 ppb 1After aeration ^Represents seasonal variation, difference from one month to the n e r t , will not exceed 10Z cAverage of all well water values from January-September, 1987 ^Total monthly range of organic carbon Sample dates: Trace elements June 3, 1987, organophosphate and organochlorine analyses May 28, 1987. 000206 ABC LABS #36616-10 BEST COPY AVAILABLE TABLE 2 Acute Toxicity oi E2566-2 to Daphnln magna Co b pound E23UC-2 LCS0 (mg/1) 24 hours >'32 (estimated) b 4ft hours (1.0-1.8)C a Bioassay conducted at 20C (i2.0). ^95" confidence limits could not be established. c 952 confidence limits. The 24- and 48-hour no-effect concentrations were 32 and 1.0 mg/1, respectively, based on the absence of mortality and abnormal effects. All values were rounded to two significant figures following the technique provided in ABC S.O.P. #8.7. LC^q calculated using: ^ B i n o m i a l Method 000297 ABC LABS #36616-11 of 48 BEST COPY AVAILABLE TABLE 3 Percent Mortality and Water Quality Measurements During the Acute Toxicity Test of E2566-2 to Daphnia m a g n a . Nominal Concentrt ion <5L Control 1 .0 ;.t a.: 5.8 10 ]t; 32 Percent Morta 1Itv 24 hr 48 hr 00 00 0 80 0 100 0 100 0 100 0 100 0 100 Temp "l 1 ) l l 19 19 Water Quality 0 hours _____ ).0. h ffg/1 ejj! 9.3 8.2 V .{4 8.2 48 hours Temp. c 20 D.O. !BZi _PiL 8.7 8.3 20 8,7 8.3 9.4 8.2 20 8.7 8.3 9.5 8.2 20 8.7 8.4 temperature - mercury thermometer. Dissolved oxygen concentrations - YSI 54 ARC dissolved oxygen meter. CpH - Corning 140 pH/mV meter with Beckman 39831 electrode. KOTE: Dissolved oxygen saturations at the test temperatures of 19 and 20C are 8.9 and 8.7 mg/1, respectively (corrected for altitudinal pressure at ABC Labs). 0002G S ABC U B S C3016-12 of 48 BEST COPY AVAILABLE LITERATURE CITED (I) CctHEittee on Methods for Toxicity Testa with Aquatic Organisms. Methods of Acute Toxicity Tests with Fish, Macroinvertebrates and Amphibians. 1975. U.S. EPA, Ecol. Res. Ser. 660/3-75-009. (Z) American Public Health Association. 1980. Standard Methods for the Examination of Water and Wastewater. 15th ed. Washington, DC. 11j*. p . (3) Pennak, R. W. 197S. Freshwater Invertebrates of the United States. John Wiley A Sons, New York, 2nd ed. 803 p. (A). Stephan, C. E . , K. A. Busch, R. Smith, J. Burke and R. W. Andrews. 1978. mental A Computer Program for Protection Agency, Calcula Duluth, ting Mi nnaensoLtCa5r,0' V, S . Env ironpre-publication manuscript, August, 197b. (5) Stephan, C. 1977. Methods for Calculating an LC^q , p. 65-8-4. In K. I.. Mayer and J. L. Mantel Ink (eds.). Aquatic Toxicology and Hazard Evaluation, ASTM Special Technical Publication 939. ASTM. Philadelphia. (b) Organization for Economic Cooperation and Development. 1981. OECD Guidelines for Iesting of Chemicals, Principles of Good Laboratory Practice Annex 2, C(81) 30(Final):7-28. 0002G9 ABC LABS (136616-13 of AS BEST COPY AVAILABLE QUALITY ASSURANCE STATEMENT Quality Assurance Statement for report <06616 entitled, "Acute Toxicity of E2566-2 to Daphnla m a g n a ," for Hr. Mohased F.lnabarawy, 3M Company, St. Paul, Minnesota. In accordance with ABC Laboratories' intent that all studies con ducted at our facilities are designed and function in conformance with good laboratory practice regulations and the protocols lor individual laboratory studies, an inspection of the final report for E2566-2 was conducted and found to be in an acceptable form by a member of our Quality Assurance Unit. A procedure audit was conducted on December 14, 1987. The study director was notified of the results on the same day. The results of this audit were reported to ABC Laboratories' management on December 30, 1987. A final inspection oi all data and records on January 14, 1988, indicated that the report submitted to you is an ac curate reflection of the study as it was conducted by ABC Laboratories. Should you have any questions relating to the information provided in this statement or the function oi our Quality Assurance Unit, please contact the Quality Assurance Unit at your convenience. Quality Assurance Officer Date 000270 ABC LABS #36616-14 of 48 's t u d y c o m p l i a n c e : s t a t e m e n t BEST COPY AVAILABLE Study Compliance Statement for ABC report 036616 entitled, "Acute Toxicity of E2566-2 to Daphnia m a g n a ," for Mr, Mohamed Elnabarawy, 3M Company, St. Paul, Minnesota. In accordance with ABC Laboratories' Intent that all aquatic toxicity teats conducted by our facility follow good laboratory prac tices, ABC's study director for the above teat herein confirms that the study was conducted in compliance with the OECD Guidelines for Testing of Chemicals, Principles of Good Laboratory Practice Annex 2, C (81) 3 U ( F i n a l ) :7-28. All original raw data were provided to 3M Company, and a copy retained at Analytical Bio-Chemistry Laboratories. Scott Frazier ABC Study Director Dace 00O2?l ABC LABS #36516-15 of 48 mimb ist copy APPENDIX - RAW DATA KOTE: Some of Che records which appear in this raw data appendix have been' provided as photocopies of original records on file at ABC. This has been done by necessity for certain data which are used commonly in several studies at ABC. Such records may include analytical standard solution preparation sheets, organism culture logs and well water chemical screen results. 000272 MCU8$#0'3bb I b PS* 00 I bof 0048 ACTIVATED SLUDGE RESPIRATION INHIBITION TEST SUBSTANCE Identity: Perfluorooctanesulfonylamido(ethyl)acetate; may also be referred to as PFOSAA, FC-128 or as the major component of FC-127, FC-129, FC-109, orFC -109-X . (Glycine, N-ethyl-N[(heptadecafluorooctyl)sulfonyl]-, potassium salt, CAS # 2 9 9 1 51-7) Remarks: The test sample is FC-109-X. Current information indicates it is a mixture of 19-23% test substance, 61% water, 12% 2- methoxymethylethoxypropanol, 2% ethanol, and 2-6% C4-C7 fluoroalkyl carboxylate compounds. Test sample was from 3M production lot 2. The following summary is abbreviated because die test sample is a mixture of the test substance in a water/organic solvent solution. Data may not accurately relate toxicity of the test sample with that of the test substance. METHOD: Methods: O ECD 209 Test type: Static acute GLP: No Year Completed: 1987 Inoculum: Activated sludge mixed liquor collected from the City of St. Paul, Minnesota Wastewater Treatment Facility. Inoculum mixed liquor suspended solids: 2.9 g/L Inoculum holding: None - used the day it was obtained Analytical monitoring: Dissolved oxygen concentrations Exposure period: 30-minutes and 3-hours Measurements: Dissolved oxygen depletion rate after 30-minutes and 3- hours of exposure. RESULTS Nominal concentrations: 2 Blank controls, 100,180, 320, 560, 1000 mg/L Element values: 30-minute EC50 = >1000 mg/L 3-hour EC50 = >1000 mg/L (5.9% inhibition at 1000 mg/L) All element values based on nominal concentrations. 0 0 2 73 Control response: The largest percent difference between control uptake rates was 4.3%; thus the two controls were within 15% of each other. Reference substance results: 3,5-dichlorophenol at a concentration of 10 mg/L induced 45% inhibition in respiration rate. This was within the normal range seen in this laboratory with this inoculum. Remarks: Testing was conducted on the mixture of the test substance as described in the test substance remarks field. The value reported applies to that mixture and not the test substance. No attempt was made to determine the impact of the presence of the organic solvents or what portion of the toxicity can be contributed to the Perfluorooctanesulfonylamido(ethyl)acetate. CONCLUSIONS The FC-109-X 3-hour EC50 for activated sludge respiration inhibition was determined to be >1000 mg/L. Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 DATA QUALITY Reliability: Klimisch ranking 2. Testing meets all criteria for quality testing, but lacks analytical confirmation of test substance concentrations. There is a lack of characterization of the test sample. Because a mixture was tested, care must be taken when interpreting the results. REFERENCES This study was conducted by the 3M Company Environmental Laboratory, St Paul, MN, Lab Request number E2113. OTHER Last changed: 5/18/00 000274 BEST COPY AVAILABLE ENVIRONMENTAL LABORATORY ACTIVATED SLUDCE MIXED LIQUOR liU L 2 J ! 3 _ _ Data Analyst ~fi Type Teat Ac I < !?-<.pi fa^lffv> Xn hi Lullova tt Jo?/ Source /j^ c c ? C<Jtv<-K. T renAm f >\f P la V i4 - f v f P a u l } M * J _________ Date Obtained 0 - % C - & 7 Date Used C ~ 3 d* ~S 7 Mixed Liquor Suspended Solids (MLSS) .*-1 k /L Adjustment .VroW b /L PHThlVVrH - t-IVjfVl = j ) Comments.____________________________________ ' ______ ________ Test SubstanceSample Description F-*- ) o 3 ' X ( H I - fro! - o H i U - c i d A Y FC S u r f a H a M Sample pH |-^ v QrwyfCt: - 7-3 Adjustment A'o h t Comments Reference Substance ; Sample Description. 3, 5 ' Icf.U.p'h t h e ! _________ Sample pH 7- ______ Adjustment X / o n i Comments .`x fr r fc fir li. X lo n .5 0 1714 I t : Exposure Conditions Test Duration 3, ^ Test Temperatur- I*1 " .3 C* C Conoscot s T u ') ( f t i U L ft. "f i d ) } Q 'BKTCflPY AVAILABLE Environmental Lab - Work Sheet C l C h A <1.4WCV\CcL S i ( or l/VC Simpl Oticription FC- 10I / (^piratien _t^h>biiicv\. T e s t ill ii/'i-iNW e . f Jo P C icU<H i uf , titl _____________________S > C 1i H I0 VI Lib R iq uilt No. 3 I 1 ***> PiO*. 1 .Of. *> Da,U: i C - 3 r - X I Analyjt:, U sV i>ro f6 '> c 1fi C: *7c 3 :lo UgO 5 /.- y. %o loco o l'int lJ i ' ^ k c U . .. O h\i, D I u:itrr* At\i\t<i./sccn*iL ivuL^y^tKetvci r>vi_ i ;\ '~ c ; X 4j ` / J it. f^ t 7. 4 + / 6 + V i'.- ) 7 . 4 < /0 t j cc <-. .? S ` f . - + . / ( f . V c F f I ( t- .V " ___ -- ---- J S 1/ 4- lb r :)CL- - o iu | w i-ytore w o tvrtte .ir e .5 c o SCO 5 'c c Set '> c & 1 J p p a r t n i ! j / .- i Y L \ v .- L 'L U L U .u k r-it:-- i r : . i H r . '/- J~niv.il-H o <-< ^ d W j . fAny.-O -Crcryi 7, I ' ( l e n f S f ^ g t ^ j t o _7 , ^ <'of(,.J \ t n.in, hfi p f) i.o o .^ t y i a f i f r ------------ --- ------------------------------------------------------------------------;_________ TT> CcUct X 1^. j,4k u m ii.7 fs C c n u d ' I Z - ft Ue4f.r\vJ Z . t'.'',li IlftL Mr<*hcn je J 7 .f ? 00'f>2^6" ENVIRONMENTAL LABORATORY LR & 2 1 X OECD ACTIVATED SLUDGE RESPIRATION INHIBITION TEST #209 RAW DATA Test Substance: R ' - /Cr1- X h i s . 3 L M - C *- ;U v" L e t ^, Source of Activated Sludge Mixed L1quor:J >\e 1fci f- C \ 'K T'r '- f ' A i ' f St Tkcl , M * J Date Received: f /*> 7 A ~ Analyst:^ ___Q j o c l . d ' x Date Used: 7 BEST COPY AVAILABLE 30 - MINUTE EXPOSURE DISSOLVED OXYGEN CONCENTRATIONS mo/1 lest Substance TIME-MINUTES TEMP Concentration (mg/L) 0.5 1.0 2.0 3.0 4.0 5.0 i 5.0 7.0 8.0 9.0 10.0 C* CONTROL I 7.V 7- X L - l ir.Z 7 . 7 s . a H. _/ */..Z 3 . 7 3 7 7 . 7 J ICC nkr. 73 r za '7 a.q 7.C .5 L-.X 5.q .5 7 4 > L- n /, ,7. "r7. *") 5.i. L - - -fT. 5' / a . r 4 f q 3- 3 7 -> 7 5- 11 H i A .3. S' 3 . c :\ n _ 3d 3.5" 2 c 30 "5 L O !C C C A HA h x (;.X L Z _ 55 lf7 M17 -"\ .A 2. 1 5 i 5' 3-7 3 5 I, I c . i - J.S .73 2b Z CONTROL II 7 . \ s L i j 5 7 1 5 5 5 . C ^1; 5- V-f 5 1 3 7 3 . 7 l 3 - HOUR EXPOSURE -^ lest Substance Concentration (mg/L) CONTROL I Io n ISO 320 lo o DISSOLVED OXYGEN CONCENTRATIONS mq/L TIME-M INUTES TEMF 0.5 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 CB 7.0 9 6 . 3 1 5 . 7 5 .1 H-t, H.O 3 . 5 7` LI 7.X 6 . 7 6 1 n 5 . 3 1 7 i L 7A * 7 Z o l a >!7) 5 h JSJL 7 1 1 5 7 h 7.-5' 7 f 1 b. 1 5 5 5 . 0 H A -?.*y H 3. G 3 J . l i z I I 3 ,6 3 1 H.o ,3 7 3 . 0 9X2 20 2o 2 7 .X i i 6 .5 * 5 1 5 1 1 1 1 1 3 .8 3 3 ?;7 l Z 7.1 5 0 5 .0 1 1 351 3 3 7 CONTROL II 7 .5 . L I . 1 L 5 1 5 \ pH of Activated Sludge Mixed Liquor; pH of highest concentration tested: Te?t Temperature: ! ^ - J U ' r C. Initial 7, M I n i t i a l 7 . tj1 000277 7 . 0 3 .H <?.s <2 . 3 5 0 Final . j Final g j'-' |>\i Cor SL-.|r., .H'cp EWIROfMENTAL LABORATORY ACTIVATED SLUDGE RESPIRATION INHIBITION TEST #209 CALCULATION OF RESULTS lr x n 3 Date U< - T o - g 7 Test Snh;ran<v F C ~ I Q M - X ( V I ~ J L-OI- C H t H- O L e t a } F C 4 U rCwg(a..Tf Pft 3 V 3 30 - MINUTE EXPOSURE Test Substance Concentration (me/L) CONTROL I IC O IR C - 370 .. 5 k O . te c e Oxygen Uptake Rate R O -5 C C C C . 5 C C C: c .scc o 7 . 5 2 M X C . M l 4 11 O s / R Ll R Corrected^ to 20* C C 5 C c C C 5<r f o r .5 c* r o C 5 . 2 `CJt C M 7 C1 H C , 5 1 `1 % Inhibition in p . Respiration Ratel"J -- -- -- -- 7. 1 -- CONTROL II C . H 5 7(- 1Percent Difference in Cont EC.q (95% Confidence Limit : `Lw, 2 - h o u r Etroamii Test Substance Concentration (mg/L) Oxygen Uptake Rate R CONTROL I ....... i i r C > !Q n o .S it, | a . .5! c . li x c c 75X0 . S L .O to c o c> . 5 1 X 5 O .574/ 0 . 5 Mx 0 M 7 4 1 -- /a t s t f i f l P Y a v a i l f t R i r R Corrected*^ to 20* C 0 5 5 1- 1 4 /V 5 C CC . 5 1 XX t 5 X 5 1 C . 5 i MR % Inhibition in p. Respiration Ratel"J -- 7.4 Ix & .i s .a , s . cl CONTROL II -- Percent Difference in C o n t r o l s ^ > , X T 1c _____ BCcq (95% Confidence Limits) mg/L__^ i .C - 4 1 2 )5 ^ .lJ = . (1) Temp. Corrections--- (mg 0 2/L-min.) i^El t a (2) % Inhibition i " * "7|ZRC1, RC. X 100 hhere: R * Oxygen uptake rate (mg 0,/L-minJ T,obs * Sample temp., C* & 1.Q47, x = T,obs - 20*C C * Control (3) I Differences 1^1 - X 100 |RC1 + RC^ The two control respiration rates should be within 15% of each other -5o < [>\ j_ -AC'r Tus+ 0 0 0 2 7 8 Soldicvv ------------------- -- iX o tV . S j l u - h o n * ___________ C .C -X "3^.L ,,., __ n n l ~ c> H Q Tv>t^c.,4i f Kfc- iv>^ 3,-v-lVP u->_i r >v< <0.A> ViOH r V t o ^ c L tt; ? o th / v.v\^lu >M. _________ " 4 U f r l , o n < r S t i r r u p I-u At llpiCy d r e p u t e . q h I i I I n o p i m t pp ~~ l u i</t -fa__ > *- < v n*v . b ^ -- ^a-lgr.:___________________ :________ - X f t i-iiAL.-p .ri .:________________ ? k avHft ^ - 7 ,^ i i & i .- $ c k . i t z * s,.Z Tm Oc ' ' " It I Ci - . ~U T & zv~ f',y *on4fls. O KT755E M . t u}a*r A,iJ^l%OCU 4lftl/>Ct.J t o :x 7 ` I -t y RvS3v5ti<VtZJ *t^S3Cmf ' It, \L rPXSvtTETT AXUxlw.vUi JCC* Co To*al Ai*w*e mi 'S C f> C t__ Cciri, t a l k - XxAxeJj.. L i'iiiV __ LK Lu%- ' t W i W VC a V 7 / Si gri d t o - a i g 7 r i\i * L .U ENVIRONMENTAL LABORATORY OECD ACTIVATE SLUDGE RESPIRATION INHIBITION TEST 1209 RAW DATA Test'Substance:, h i d i l - t r p U i v : l ftOret-u 8 u b c , i m ^ i _____________ Source of Activated Sludge Mixed Llquor:>ltArtJ Ja^AjL-IfgaAmlnt F * M *J Oate Received: JO - ^C> - & 7 Date Used: K 1- .7n -.3 ~7 Analyst:A 30 - MINUTE EXPOSURE lest Substance "TTmT MINUTE TEMI Concentration (aig/L) 0.5 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 C' CONTROL I m 7.4 7. -J. U. 7 . .2 S r 7 5 , a 4 .7 4 . a /.7 3 . J 2 . 7 7 - 1 7- eqM . 0 5 .8 H A 3.<* 3 CONTROL II A If A u J15 ^ s . s 5 / 0 '/ . I 3 . t 3 . <3-1 HOUR EXPOSURE lest substance Concentration (mg/L) 0.5 CONTROL I 7 .0 / 1.0 2.0 . 9 it .3 7# 3.0 t Im -n INUTE5 4.0 5.0 6.0 7.0 8.0 9.0 10.0 TEMF C* 5 -7 5 ` i H-b H.o 3 .5 r A 30 7 - 5 7 3 , 4 . T (> A V, 5 e! 5 . t S A V . -, .. , ., .. * . ...; . *' CONTROL II 7 ? Zi. .1 S A 5 . 1 M pH of Activated Sludge Mixed Liquor: Initial 7-*i Ptl f highest concentration tested: Initial 7,U Test Tenperature: I V 3 \<L 000280 , y . & L 3 .S Final & I Final / c j 3o * * c ( > ^ 4 . e r lc<vt i>c U > . p ( V p ACTIVATED SLUDGE RESPIRATION INHIBITION TEST 209 CALCULATION OP RESULTS Te st S u b s t a n c e t i l , .-l2 .fe .ffri(C . 30 - MINUTE EXPOSURE Test Substance Concentration (mc/Ll crwrnnr i ' to Oxygen Uptake Rate R O .s o c o c . 7 > lc '^ R Corrected^ to 20*C O . 5 0 0 c) .Z ~ to ? > lr c a u.J ~ Date J , C : , l C r 2 An alyst ^ *3 1 Inhibition in , 7) Respiration Rate'-4'1 -- AH CONTROL II o . __________ Percent Difference in Coni.rols^ 4 - 3 EC jq (951 Confidence Limit m o / t I t 7 m a I L ___ i 3 - m m pvpoigmp Test Substance Concentration' (mg/L) CONTROL I tn Oxygen Uptake Rate R O S H lei 0 . 4 7 cl l R Corrected^ to 20*C 0 . 5 4 61 C> . ? > C O H - -- I n V ^ V i U l t m ___ ___ 1 Inhibition in Respiration Rate14-' 4s ~ r CONTROL II ^ 547V 0 .5 *4 7 3 Percent Difference in Controls^ - 3 ___________ BCSQ (951 Confidence Limits) mg/L IC P / \ 1 (- !n ^ f / i , . -- y i v ;:; j y . f1 ( 1J T top. C o r r e c t i o n s 1 1 ' ^ S| (mg 0 9/ L - n i n . ) (3) 1 Difference - " X 100 fa * ^ (2) I Inhibitions*'/ .. . ^ * X 100 , fcc1 BC^ hhere: t' l 4 R Oxygen uptake rate (sag 02/L-min.) T,obs Sample temp., C* ft- 1.047, x - T,obs * 2(fC C Control 000281 The two control respiration rates should be within 151 of each other 9 ^ 4 . " i o r .5sYoclc 4 i-f&kt y *v -tt i V *v-viVr-> - r f . ' i .j ,,..'* MICROBIOS MICROTOX TOXICITY TEST TEST SUBSTANCE Identity: Perfluorooctanesulfonylamido(ethyl)acetate; may also be referred to as PFOSAA, FC-128 or as the major component of FC-127, FC-129, FC-109, orFC-109-X. (Glycine, N-ethyl-N[(heptadecafluorooctyl)sulfonyl]-, potassium salt, CAS # 2 9 9 1 51-7) Remarks: The test sample is FC-109-X. Current information indicates it is a mixture of 19-23% test substance, 61% water, 12% 2methoxymethylethoxypropanol, 2% ethanol, and 2-6% C4-C7 fluoroalkyl carboxylate compounds. Test sample was from 3M production lot 2. The following summary is abbreviated because the test sample is a mixture of the test substance in a water/organic solvent solution. Data may not accurately relate toxicity of the test sample with that of the test substance. METHOD: Method: Microbios Microtox "BASIC" Procedure Test type: Static acute GLP: No Year Completed: 1987 Species: Photobacterium phosphoreum Analytical monitoring: None Statistical methods: EC20, EC50, and ECso values calculated by statistical linear regression program provided for Microbics Microtox system. Test organism source: Microbics Microtox reagent Test conditions: As per Microbics Microtox method Replicates: Two RESULTS Nominal concentrations: Blank control, 125, 250, 5 0 0 ,1 0 0 0 mg/L Element value: 5-minute EC20 = 1 7 0 mg/L 5-minute EC50 = 650 (560-750) mg/L 5-minute ECso = >1000 mg/L 15-minute EC20 = 140 mg/L 15-minute ECso = 4 1 0 (320-530) mg/L 15-minute ECso = >1000 mg/L All element values based on nominal concentrations. 000282 Remarks: Testing was conducted on the mixture of the test substance as described in the test substance remarks field. The value reported applies to that mixture and not the test substance. No attempt was made to determine the impact of the presence of the organic solvents or what portion of the toxicity can be contributed to the Perfluorooctanesulfonylamido(ethyl)acetate. CONCLUSIONS The FC-109-X 15-minute EC50 for Photobacterium phosphoreum was determined to be 410 mg/L with a 95% Confidence Interval of 320-530 mg/L. Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 DATA QUALITY Reliability: Klimisch ranking 2. Testing meets all criteria for quality testing, but lacks analytical confirmation of test substance concentrations. There is a lack of characterization of the test sample. REFERENCES This study was conducted by the 3M Company Environmental Laboratory, St Paul, MN, Lab Request number E2113. OTHER Last changed: 5/18/00 000233 Toxicity c> F C - ( 41- 113 - om 14-o Lot a ) S4P> To AUCrobicil Sy,S+<2rvvS BEST COPY AVAILABLE Test Gone. nnt I I A\iCCQ tO'X Perce nt Li^'nt t-uixS 5-*1*4 E.r> f5 >1(.V txr* IJ 5 *3 5 ?5o 7 ,5 as 5oo H1 3 1o o o fc3 7C1 C?.o ^ 5 0(45% Cl\) ! 70 G5o fofco- /So) 140 4/0 (3^c-530) iC So V/oco )lfico T ^n C5t Lon C . Percent I n h i b i t i o n loo /go 3^.0 560 /ooo -- -- --, 1 -- ^C(455 5cC l)v > I00O 5.4 IX 6.1 . 3.2 5.=! > /coo 0002B4 * LR jE _ana_ P l c > ^ RAW DATA T ES T s i H K T W F - F C - i O q - X ( m - 2 .L'CI-_ M 1M-C ..Let- 3 ^ -- C - ~ j u d a c f o r! f_____ TEST DATE: I - i S S 7 IA N A LY S T : t2clcl\ SAMPLE CUVETTE 81 Cl FINAL ASSAY CONCENTRATION YVu< / o "T iiT T T T " READING KO) BLANK CONTROL DUPLICATE Ho HH FIf LADING! 5-MIN. 15-MI H. 30-MIfl. K 5 ) 1(15) 1130)__ b$ S 7b i 82 C2 D u p l c a t e HH 6 *7 Ico 6 7 46 H6 83 ; 5 ' c C3 b c p lic le . <H7 7 HH Hb 5 H H! Ok 4C*D Sea Ib u P lic rtV e HH 4 3 31 I c o HH 3 / 85 l o c o HH 7 7 I * C5 . -A'; b u p l a ie HH 7 3 13 T<tr* Sk*b^v<vv\c<. % m)*CCf- SCf^'Tl L'inKc^t A p ft\rrv V ly ^ u s c i t a l i - o J l t k H i i t i f . S + o c t b i o t i c Vi,x*> cunt- C o t e r - Cclc-r n w- a p ftar Q v t ^ h yW e S* C e n e . . | c e -* E'rtf * 7 .3 , d j ^ ^ eAl.; ? i f 4.7 tv .-i-U t v / 4 , sc4 ^ W j v h w . t o . U C C ic jc^ pH ^ j ^ K c i S a ^ , ^i vi cr_ r.bls _. % /U ^a . S ^ * )ch 0002S5 J. vittial ; I,,; b Wdkr u W tc ^ e r T>.s+nJ IC .^-g7 Aer*.Mc.A ( so/ . j .ntc- t i , . ru .c L I(o a ,, J ;-/i-fl7y p/f-4-C AVAILABLE MICROBIOS MICROTI-OX11 SYSTQ-I LR J? 113 U1.Q.-I&-87 MICROTOX DATA REDUCTION Analyst_SJL_____ F C -1 lH i' 2i>cl-cyiti-c u t- z ) B U N K RATIOS* BLANKCBC1lU..V..E.T..T..E... Html PC S u r C a d Initial 1IB*hLAcN-KOR.TA5-TSMTtOI,N. DIFFERENCE 6'. C'i A -an t -----------15_ H T BtyNK rVn-g JRUAaTlfIlOc . irD-I-F-F-E--R-E--N--C-E-o. cos' 5 PA p-reopr. SfccV. --B-L-A--N-K---R-3ATI-OHIND.-I-F-F--E-R--F-N--C--E- *The blank r a t i o s fo r B1 and Cl should agree w ithin 0.02. MEAN BLi^K RATIOS Bl BK RATIO Cl BK RATIO 2 . I ............ ............. ft-.5-1M*I2N.,_________ _______ o IS--MIN.__________ b tH ______ 30-MIN-_________ NORMALIZED LIGHT LOSS (PEFFECT) Mean Blank Ratio x Initial Sample Reading Final Sample Reading SAMPLE CUVETTE 5-M IN. P Test Concentration o. A I7 B2 C2 i 2 5 ~ *t<\)L lu - : : .^ . C3 %SC> O . 221 o 317 o 3.5.5" B4 C4 S o o C.. blob o 71-x BS /. bi >3> C5 l OOO ___ L -JH H ______________ 1 5-M IN. r o. 3 a i 0 .3 3 5 " o- 35*/ O 1 35? O. fc^ o .q s l 3 S l O 3 - b i b ____________ 30-MIN. P Z LIGHT LOSS (ZA ) - -- C -- X 100 i+r STAeMsPtLECoCnUcVeETnTtrEation CBBCCBC5432453 ) US' ASO. 500 OO ^P \ 5-MIH. Z A is -2Hi*xo3U _____________________ _ A1H5-MIN. Z A 5 3u b0 30 771q 30-MIN. Z n EFFECTIVE CONCENTRATIONS (EC'aU O ^ J j:____^Calculated using "P,C" data oairs.) EC'S 5-MIN. 1C20 lu b tCrn (95Z Confid. Limits) ~~ 50 ^ (5>^-7^o) iE80 > i c o o 15-MIN. 30-MIN. HH H iZ f 3 J i ~ S 3 a ) > toco 7 T