Document X8Dy97qKXNg3g744yNJZYyyBy

ACUTE TOXICITY TO FISH (FATHEAD MINNOW) TEST SUB TANCE Identity:A mixturecontainingperfluorooctanesulfonawthei,ch may also be referredtoas PFOS, FC-95, or as a component of FC-600. (1-Octanesulfoniaccid,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8heptadegafluoro-p,otassium saltC,AS # 2795-39-3) Remarks: The 3M productionlotnumber was notnoted. The test sample isFC-600 (BelgiumAFFF). Currentinformatioinndicatesitisa mixtureof 1.0% PFOS, 81.20% water,12.00% diethyleneglycolbutyl ether,1.00% sodium octylsulfate2,.00% propane Sultonefoamer, 1.00% sodium decylsulfate0,.85% xanthan gum, 0.1% N-(3-chloroallyi) hexaminium chloride0,.80% starch,and 0.05 % tolyltriazole. The followingsummary applies to a mixture with incompletely characterizedconcentration of impurities.Data may not accurately reflectthe toxicityof the fluorochemical component of the test sample. METHOD: Method: Procedures closelyfollowedthose outlinedinEPA-560/6-82- 002, OECD, and ASTM Proposed standardpracticesforconductingacute toxicittyestswithfish,macroinvertebratesand amphibians,E729-80. Test type:Acute flow-through GLP: No Year Completed: 1982 (study)and 1983 (report) Species::Pimephalespromelas Supplier:Commercial supplieirnBrady,Nebraska. Analyticalmonitoring:Temperature,pH, and DO Exposure period:96-hours Statisticamlethods: LC50 valuesand 95% confidenceintervalcsouldnot be calculated.There was no mortalitdyuringthe test. Test fishage: Juveniles Average Length and weight: Lengtl-=i3.8 + 0.45 cm Weight = 0.42 + 0.11 g Loading: 0.47 g/L Pretreatment:Not noted. Test conditions: Dilutionwater: Carbon-filterewdellwater,3M well#2, St.Paul, MN. Dilutionwater chemistry: Dissolved Oxygen: 95 - 98% saturation pH: 7.9-8.1 Hardness (asCaC03): 250 mg/L Alkalinit(yasCaC03): 230 mg/L Conductivity: 340 pmhos/cm Lighting;Coolwhitefluorescenltightpsrovideda dailyphotoperioodf16 hours lightand 8 hours dark witha 30 minute transitiopneriodwas maintained duringtesting.Intensitwyas measured at 60 - 70 foot-candles at the water surface. Stock and testsolution preparation: A 40,000 mg/L stock solutionwas prepared dailyby dilutin2g40 grams of testsample to 6-L with dilution water. Test solutionswere prepared by a dilutedreliveringfivenominal concentrationof the testsample and controlwater. Flow-through rate: Approximately fivevolume replacements per 24 hour period. Stabilityof the test chemical solution: Not noted. Exposure vessels: 24 cm diameter by 25 cm deep cylindricagllass aquaria with a maintained testsolutionvolume of 9 liters. Number of replicates:two Number of fish per replicate:10 Number of concentrations: 5 plusa blank control Water chemistry during the study: pH range (0-96 hours): 7.5 - 8.2 (controlexposure) 7.5- 8.2 (1,000mg/L exposure) Temperature range (0-96hours): 18 - 200C (forallaquaria) Dissolved oxygen range (0-96hours): 6.7- 9.0 mg/L (controelxposure) 6.1 - 9.0 mg/L (1,000mg/L exposure) RESULTS Nominal concentrations: Bk control1,00, 280, 320, 560, and 1,000 mg/L Percent mortality (based on 20 fish per concentration) Nominal Concentration (mg/L) Control 100 280 320 560 1000 24-hours Percentage mortality 48-hours 72-hours 0 0 0 0 0 0 1010 0 0 010 0 0 0 0 0 0 96-hours 0 0 0 0 0 0 Element value: 24-hour LC50: 48-hour LC50: 72-hour LC50: 96-hour LC50: >1,000 mg/L >1,000 mg/L >1,000 mg/L >1,000 mg/L Element values based on nominal concentrations. Remarks:Testinwgas conducteodn themixturaesdescribeidntheTest Substance Remarks field.The value reportedappliestothatmixtureand not the fluorochemicalproportionalone. No secondary effectswere observed duringthe 96-hourflowthrough test. CONCLUSIONS The FC-600 96-hour LC50 forPimephales promelas was determined to be >1,000 mg/L. Submifter: 3M Company, EnvironmentalLaboratory,P.O. Box 33331, St. Paul,Minnesota,55133 DATA QUALITY ReliabilityK:limischranking2. The studymeets allcriterifaorquality testing.However, the sample puritywas not propedy characterizedand the studylacksanalyticaclonfirmationofthe amount offluorochemical proportioninthe solutions. REFERENCES This studywas conducted by the 3M Company, Environmental Laboratory,St.Paul,MN, 3M Lab Request number 9595, 1982. 3M TechnicalReport "AquaticToxicityTesting:FC-600 (Belgium-AFFF) LR 9595."M. T. Elnabarawy, Project9970012600, Commercial Chemicals, Report Number 82, July21, 1983 OTHER Last changed: 6/28/00 Form 6747-1I-E TECHNICAL REPORT SUMMARY TO: TECHNICAL COMMUNICATIONS CENTER - 201-2C-12 (Importan-tIfreporitsprinteodn bothsidesofpaper,sendtwocopiestoTCC.)Guidelinoens reversseide. Division Environmental Laboratory Project Commercial ReportTitle Chemicals Aquatic Toxicity Testing: To (EE & PC) FC-600 (Belgium-AFFF) Author(s) M. T. Elnabarawy Notebook Reference LR 9595 Dept Number 0535 ProjectNumber 9970012600 Report Number PeriodCoveredor Date 7/21/83 Employee Number(s) 46981 No. of PagesIncludingCovershoot SECURITY 10KEYWORDS: Lab Code OtherKeywords Open Report& Summarv 0 ClosedResmrt-Open Summary CURRENT OBJECTIVE: To determine the acute varying concentrations through conditions. 3M CHIEMICAL REGISTRV P' I Check box ifnow chemicalsarereported.Use Chet calRegistrFyorm 6092 toreportallnew substanc@ aquatic LC following of FC-600 @gelgium-AFFF) exposure to under f low- EE & PC-Div. (Env. Lab) Toxicity (Aquatic) REPORT ABSTRACT: ThisabstracitnformatiiosndistributbeVdtheTechnicaClommunicationCsentertoaler3tM'ers Company R&D. The acute aquatic 96-hour LC values obtained for fathead minnows (Pimephales promelas@ofollowing exposure to FC-600 in replicated experiments were greater than 1,000 mg/l under flow-through conditions. The acute toxicity of FC-600 to aquatic organisms was considered insignificant under the reported test conditions. nformation :nitials: Liaison ACUTE TOXICITY OF FC-600 (Belgium-AFFF) FATHEAD MINNOW (.Pimephales promelas) UNDER FLOW-THROUGH CONDITIONS LR No. 9595 (9970012600) Prepared by: M. T. Elnabarawy Sr. EcotoxiCologist Environmental Laboratory EE & PC 3M Company - 2-3E July 20, 1983 INTRODUCTION The purpose of this study was to estimate the acute toxicity of FC-600 (Belgium - AFFF) to fathead minnow (Pimephales promelas) under flowthrough conditions. Preliminary range-finding static tests and a subsequent 96-hour flow-through test were conducted at the Environmental Laboratory, 2-3E, St. Paul, Minnesota. The acute toxicity of FC-600 was measured by estimating the LC50 value for the compound at each 24 hour tnterval of the test. The LC50 is defined as the concentration of the test compound in dilution water which caused mortality of 50% of the test animal population at the stated exposure interval. The flow-through test was conducted from July ll-.15, 1983. The data reported herein are based on studies performed by M. T. Elnabarawy and R. R. Robideau. All raw data generated are stored at the above location. MATERIALS AND METHODS Procedures used in this a-eute toxicity test closely followed those described in the U.S. EPA protocol entitled "Environmental Effects Test Guidelines" (1982). Other test protocols considered particularly pertinent are listed in the reference section: ASTM-E729 (1980), OECD (1981). Values are reported to different levels of significance depending on the accuracy of the measuring devices involved in any one process. The sampel of FC-600, a viscous amber liquid, was received on September 15,@ 1982. The test material was stored in the dark at ambient temperature (210 C). The material was tested as 100% active ingredient. "Nominal" test concentrations are reported as milligrams of FC-600 per li@er of test solution (mg/1). The fathead minnows (Env. Lab Lot 2-1983) were obtained from a commercial fish supplier in Brady, Nebraska, and held in a 475-1 fiberglass tank under.a photoperiod of 16 hours light and 8 hours darkness with a 30-minute transition period. All fish were fed a basic dried fish food, Tetra Min, daily except during the 48 hours prior to and during testing. There was less than 3% mortality in the test fish population during this 2-day acclimation period. The temperature in the holding tank was 20+1 0 C during this 2-day period (Daily Record of Fish Holding ConditionsT. The well water which flowed into this-tank was characterized as having total hardness and alkalinity ranges as calcium carbonate (CACO 3 ) of 250 mg/l and 230 mg/l, respectively, and a specific conductance of 340 micromhos per centimeter (umhos/cm) (Monthly Water Quality Analysis Logbook). Other parameters monitored in the holding tank were a pH range of 7.9-8.1,.a dissolved oxygen (DO) range of 95-98% of saturation and a flow rate of a minimum of 2 tank volume replacements/day (Daily Record of Fish Holding Conditions). Test fish were maintained under these conditions for a minimum of 14 days. The specific conductance was measured with a YSI Model #31 conductivity- bridge, the pH was measured with an Orion Model 407A pH meter and combination electrode, the DO was measured with a YSI Model #54 dissolved oxygen meter and probe and the temperature was measured with an ASTM-Calibrated thermometer. Total hardness and alkalinity were measured according to APHA et al. (1980). FC-600 Page 2 July 22, 1983 The toxicant-delivery system used in this study was a modified, (ACE Glass gas driven siphon type), proportional diluter similar to that described by Mount and Brungs (1967) with a 0.05 initial dilution factor. The bioassay diluter was constructed primarily of glass, #316 Stainless Steel, and perfluorocarbon plastics (Teflon). The dilution water was well water which was pumped to a polyethylene constant-head reservoir box where it was aerated with filtered air. This'water was characterized as having total hardness and alkalinity ranges as CACO 3 of 250 mg/l and 230 mg/l, respectively, a pH range of 7.9-8.1 and a specific conductance of 340 umhos/cm (Monthly Water Quality Analysis Logbook). A complete list of the physical/chemical characteristics of well water at.the Envir. Lab facility, 2-3E is attached. The bioassay diluter was calibrated to deliver five nominal logarithmic concentrations of FC-600; 1000, 560, 320, 180, 100 mg/l and control water containing no FC-600 to duplicate test aquaria. Each cylindrical glass test aquarium measured 24 cm in diameter and 25 cm deep with 21 cm high drains which maintained water volumes of 9 1. The diluter delivered 0.2 1 of test water to each aquarium at an average rate of 225 cycles per day. This is equivalent to 5 aquarium volume replagements per 24-hour period. Illumination was provided by Cool White fluorescent lights for 16 hours mueasuring .60-70 footcandles at the water surface each day. Test temperature was continuously monitored in one of the control tanks during the 96-hr exposure test using a Taylor temperature chart-recorder. A 10-1 polyethylene bottle was utilized to deliver the toxicant stock solution to the mixing chamber of the diluter with every cycle. The stock solution of 40,000 mg/l was prepared daily by adding 240 grams of FC-600 and diluting to 6,000.ml. A total amount of 960 grams of *FC-600 was used during the continuous flow study. After establishing the desired test concentrations in the test aquaria, the FC-600 stock solution was introduced into the diluter and cycling began on July 11, 1983. The test was initiated when ten fathead minnows uniform in size and age with a mean (N = 10) wet weight and total length of 0.42+0.11 grams and 3.8+0.45 cm (Fish Weights and Lengths Log) were rai@domly distributed 'Eoeach aquarium. A total of 20 organisms were exposed to each concentration. The fish loading ratio was calculated to be 0.47 g fish per liter of test solution. No aeration of test solutions in all test chambers was provided during the test. The pH, temperature and dissolved oxygen (DO) concentrations were measured at 0, 24, 48, 72, and 96 hours in'both replicates of all concentrations including those of the control. Biological observations of the fish including mortality and secondary effects (behavioral observations) were made and recorded daily. The general operation of the bioassay diluter was checked at least twice daily throughout the test. FC-600 Page 3 July 22, 1983 The concentrations tested and the corresponding mortality data derived from the toxicity test were'used to estimate 24-, 48-, 72-, and 96-hour median lethal concentrations (LC50). When applicable, the method of calculation selected is determined by the characteristics of the data base (i.e., presence or absence of test concentrations causing mortality of 100% of the test animal population, test concentrations causing mortality of a partial number of animals in the population,' etc.). RESULTS The test mate.rial FC-600 was not acutely toxic to fathead minnows at nominal concentrations as high as 1,000 mg/l (Table 1). No FC-600 related mortality of fisii exposed to 1,000 mg/l was observed during the 96 hour exposure period. The exposed fish appeared generally healthy and active. The estimated LC50 values after 24, 48, 72, and 96 hours of exposure were >1,000 mg/l, the highest concentration tested. No control organisms died or showed signs of disease or stress during the test. The temperature in various aguaria ranged from 19-21 0 C during exposure, and did not vary more than 2 C in any 12-hour period. The pH and dissolved oxygen concentrations measured during the toxicity test are presented in Aquatic Toxicity Data Sheets (attached). The pH levels remained relatively unchanged, and the dissolved oxygen concentrations did not fall below 60% saturation. The results lead to the conclusion that FC-600 (Belgium-AFFF) is not acutely toxic to the aquatic.environment as a result of exposure*under comparable conditions. REFERENCES APHA, AWWA, WPCF. 1980. Standard methods for the examination of water and wastewater. 15th Edition, Washington, D.C., 1134 pp. ASTM-Standard Practice, 1980. Standard Practice for Conducting Acute Toxicity Tests with Fishes, Macroinvertebrates, and Amphibians. American Society for Testing and Materials, Philadelphia, PA, ASTME729-80. Lemke, A. E., W. A. Brungs construction and operation EPA-600/3-78-072. and B. J. Halligan. of toxicity-testing 1978. Manual for proportional diluters. Mount, D. I. and W. A. Brungs. 1967. A simplified dosing apparatus for fish toxicology studies. Water Res. 1: 20-29. OECD. 1981. Guidelines for Testing of Chemicals. Organization for Economic Cooperation and Developmente Washington, D.C. U.S. EPA. 1982. Environmental Effects Test Guidelines. 82-002. EPA 560/6- Table 1. Concentrations tested, corresponding percentage mortalities of fathead minnow (Pimephales pr6melas) exposed to FC-600 under flow-through conditions. Twenty fish were exposed to each concentration. Nbminal -Concentration (mg/1) 1000 560 320 180 100 Control LC 50 (mg/1) 24 hour Percentage Mortality 48 hour 72 hour 96 hour 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 >1,000 >1,000 >1,000 >1,000 WELL WATER ()UALITY SAMPLE DATE: 6/25/83 SAMPLE TAKEN: 3m Bldg. 2-3E, St. Paul SAMPLE DATE 6/25/83 (TAKEN FROM ROOM 5) PARAMETER pH Residual Chlorine Ammonia Nitrogen Conductivity N-Alkalinity Total Solids Total Hardness Total Fluoride Dilute COD Total Coliform Standard Plate Count Aluminum as Al* @Arsenic as As* Boron as B* Cobalt as Co* Copper as Cu* Chromium as Cr* Cadmium as Cd* Iron as Fe* Nickel as Ni* Lead as Pb* Silver as Ag* Zinc as Zn* Mercury as Hg* PCB'S* Total Organochlorine* Pesticides Total Organophosphorus* Pesticides *Sample Date 3/10/83 CONCENTRATION 7.9 <0.02 mg/l <0.1 mg/l as N 340 umhos/cm at 230 mg/l as CaCo 280 mg/l 250 mg/l as CACO <0.02 mg/l <0.4 mg/l Negative 40 per ml 0 25 c 3 3 <19 ug/l 1 ug/l 15 ug/l <5 ug/l <3 ug/l <2 ug/l <0.1 ug/l 11 ug/l <7 ug/l <1 ug/l <5 ug/l 89 ug/l 0.7 ug/l <0.01 ug/l <0.01 ug/i <0.01 ug/l ENV. LAB WATER OUALITY BOOK REF. 8 9 8 9 8 8 8 9 9 10 10 16 16 16 16 16 16 16 15 16 16 16 15 16 17 17 17 ENVIRONMENTAL LABORATORY AQUATIC TOXICITY DATA SHEET DEFINITIVE (FULL-SCALE TEST) LR )e Te-s M6WIaterial Tested AELEm-CU43M@LOt ;t Organi@ininarm)-gimin.1--souMe j.Wt._0,6L-,grams Avg. Size _,@cm __Date Rec Id UZ - I Batch No. Organ3.sms per dose &) Loading Factor 3h Disease Treatment:_ ffa@E 3t SolutionVolurne@l-r-iters/All-GlasTsank Tank DimezLsions: 35x2O an and 25 an deep ie Started_-V- @@@Date Star.ted Date Canpleted -ution Water Carbon-filtered well water (Tenp. C. , D.0. restigator ill sicjl@--:7' (C)"/ LC 50 (95%-(@-onifde-ice Limits) ppm, pH g/i ink Initial Thtal Conc. Ammt mgll Added Control 24 Hours Total No. pH Dead ri 48 Hours 72 Hours 96 Hours D.O. Total No. pH ID.O. Total No. pH D.O. Total No. pH D.O. pprn Dead ppm Dead pprn Dead PPM /,//,Yg,S 0 C, IL 1,&1&,7 %.< L4:2 est Terrp. OC :nitials & Date nien -ondary Effects (other than Mortality): nk JO. Syriptans or Reactions itrol 24-Hr. 0(7 EC50 TotaT-N= 48-Hr. Af?ected 72-Hr. 96-Hr. )e Te-s 3t Organim&&WggaA&&le4) ENVIRONMENTAL LABORATORY AQUATIC TOXICITY DATA SHEET DEFINITIVE (FULL-SCALE TEST) MZSO Material Tested-24P@-@- Source Date Rec Id LR_!5? @000 Batch Wt. ,@cjrarrtsAvg. Size_S!Ld_cm No. OrganLsms per dose_ZD_Ioading Factor g/i 3h Disease Treabwmt: &Oxkt-l 5t Solution Volume q Liters/All-Glass TarLk Tank Dimemions: 35x2O an and 25 an deep ie Started_y,&I!@e Date Started Date Canpleted ,_I-@@. 'L ut.LonWater Carbon-fi-ltered well water (Temp. /6 C. D. 0. lo ,restig@ator LC5 0 (95% Cc)nfidence Limits) Ppm, pH_ZL_) iZi@2410 ink Initial Thtal 3. Gonc. knotmt nig/l Added 24 Hours Total No. pH Dead 48 Hours D.O. Total INHo. pH ppm Dead 72 Hours D.O. Total No. PHID.O. Tota @pmp$r0Dn'eadDead pgn 96 Hours Total No. pH D.O. Dead PPM 10,91 0, T,)@@ -iioo res t Terrp. OC rnitials & Date .m-ents: @ordary Effects (other than Mortality): uik \10. Symptcms or Reactions itrol 24-Hr. Z?4 EC50 Total Nud)er AfFectecl 48-Hr. 72-Hr. 96-Hr.