Document ppdxjvEGZgbEagwZLRyvLb2XB

A ft. 3.6 - 0 & < f ACUTE TOXICITY TO FISH (FATHEAD MINNOW) TEST SUBSTANCE_______________________________________________ Identity: A mixture containing perfluorooctanesulfonate, which may also be referred to as PFOS, FC-95, or as a component of FC-600. (1-Octanesulfonic acid, 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8heptadecafluoro-, potassium salt, CAS # 2795-39-3) Remarks: The 3M production lot number was not noted. The test sample is FC-600 (Belgium AFFF). Current information indicates it is a mixture of 1.0% PFOS, 81.20% water, 12.00% diethylene glycol butyl ether, 1.00% sodium octyl sulfate, 2.00% propane Sultone foamer, 1.00% sodium decyl sulfate, 0.85% xanthan gum, 0.1% N-(3-chloroallyl) hexaminium chloride, 0.80% starch, and 0.05 % tolyltriazole. The following summary applies to a mixture with incompletely characterized concentration of impurities. Data may not accurately reflect the toxicity of the fluorochemical component of the test sample. METHOD:_______________________________________________________ Method: Procedures closely followed those outlined in EPA-560/6-82- 002, OECD, and ASTM Proposed standard practices for conducting acute toxicity tests with fish, macroinvertebrates and amphibians, E729-80. Test type: Acute flow-through GLP: No Year Completed: 1982 (study) and 1983 (report) Species: :Pimephales promelas Supplier: Commercial supplier in Brady, Nebraska. Analytical monitoring: Temperature, pH, and DO Exposure period: 96-hours Statistical methods: LC5ovalues and 95% confidence Intervals could not be calculated. There was no mortality during the test. Test fish age: Juveniles Average Length and weight: Length = 3.8 + 0.45 cm Weight = 0.42 0.1 1 g Loading: 0.47 g/L Pretreatment: Not noted. Test conditions: Dilution water: Carbon-filtered well water, 3M well #2, St. Paul, MN. Dilution water chemistry: Dissolved Oxygen: 95 - 98% saturation pH: 7 . 9 - 8 . 1 Hardness (as CaCOa): 250 mg/L Alkalinity (as CaCOa): 230 mg/L 002057 Conductivity: 340 pmhos/cm Lighting: Cool white fluorescent lights provided a daily photoperiod of 16 hours light and 8 hours dark with a 30 minute transition period was maintained during testing. Intensity was measured at 60 - 70 foot-candles at the water surface. Stock and test solution preparation: A 40,000 mg/L stock solution was prepared daily by diluting 240 grams of test sample to 6-L with dilution water. Test solutions were prepared by a diluter delivering five nominal concentration of the test sample and control water. Flow-through rate: Approximately five volume replacements per 24 hour period. Stability of the test chemical solution: Not noted. Exposure vessels: 24 cm diameter by 25 cm deep cylindrical glass aquaria with a maintained test solution volume of 9 liters. Number of replicates: two Number offish per replicate: 10 Number of concentrations: 5 plus a blank control Water chemistry during the study: pH range (0-96 hours): 7.5 - 8.2 (control exposure) 7.5 - 8.2 (1,000 mg/L exposure) Temperature range (0-96 hours): 18 - 20C (for all aquaria) Dissolved oxygen range (0-96 hours): 6.7 - 9.0 mg/L (control exposure) 6.1 - 9.0 mg/L (1,000 mg/L exposure) RESULTS________________________________________________________ Nominal concentrations: Bk control,100, 280, 320, 560, and 1,000 mg/L Percent mortality (based on 20 fish per concentration) N om in al C o n cen tratio n (m g/L) C ontrol 100 280 320 560 1000 24-h o urs 0 0 0 0 0 0 P e rc e n ta g e m o rtality 48-h o urs 7 2 -h o u rs 00 00 00 00 00 00 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 9 6 -h o u rs 0 0 0 0 0 0 Element values based on nominal concentrations. 002058 Remarks: Testing was conducted on the mixture as described in the Test Substance Remarks field. The value reported applies to that mixture and not the fluorochemical proportion alone. No secondary effects were observed during the 96-hour flow through test. CONCLUSIONS__________________________________________________ The FC-600 96-hour LC50 for Pimephales promelas was determined to be >1,000 mg/L. Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 DATA QUALITY__________________________________________________ Reliability: Klimisch ranking 2. The study meets all criteria for quality testing. However, the sample purity was not properly characterized and the study lacks analytical confirmation of the amount of fluorochemical proportion in the solutions. REFERENCES___________________________________________________ This study was conducted by the 3M Company, Environmental Laboratory, St. Paul, MN, 3M Lab Request number 9595, 1982. 3M Technical Report "Aquatic Toxicity Testing: FC-600 (Belgium-AFFF) LR 9595." M. T. Elnabarawy, Project 9970012600, Commercial Chemicals, Report Number 82, July 21, 1983 O T H E R ________________________________________________________ Last changed: 6/28/00 00205 Form6747-1i-E TECHNICAL REPORT SUMMARY TO: TECHNICAL COMMUNICATIONS CENTER - 201-2C-12 (Im portant -- I f report is printed on both sides o f paper, send two copies to TCC.) Guidelines on reverse side. Division Environmental Laboratory (EE & PC) Project Commercial Chemicals Report Title -- ---- "" Aquatic Toxicity Testing: FC-600 (Belgium-AFFF) To .9iE^A's'^Reiner^t* Author(s) M. T. Elnabarawy Notebook Reference -- LR 9595 Dept. Number 0535 Project Num ber 9970012600 Report Number fz-- Period Covered or Date 7/21/83 Employee Number(s) 46981 No. o f Pages Including Covershee SECURITY KEYWORDS: Lab Code 5 Open Report & Summary O Closed Report--Open Summary 3M C H E M IC A L R E G IS T R Y Check box if new chemicals are reported. Use C cal Registry Form 6092 to report all newsubst. CURRENT OBJECTIVE: To determine the acute aquatic LC5D# following exposure t varying concentrations of FC-600 TBelgium-AFFF) under flc through conditions. Other Keywords EE & PC-Div. (Env. Lab) Toxicity (Aquatic) REPORT A B S TR A C T: This abstract information is distributed by the Technical Communications Center to alert 3 M ' Company R&O. The acute aquatic 96-hour LC,. values obtained for fathea minnows (Pimephales promelasTrollowing exposure to FC-6C in replicated experiments were greater than 1,000 mg/1 under flow-through conditions. The acute toxicity of FC-600 to aquatic organisms was considered insignificant under the reported test conditions. i Information Liaison lnitials_ _ M . 0020G0 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 ooza&L INTRODUCTION The purpose of this study was to estimate the acute toxicity of FC-600 (Belgium - AFFF) to fathead minnow (Pimephales promelas) under flow through 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 interval 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 11-15, 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 acute 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 (21C). The material was tested as 100% active ingredient. "Nominal" test concentrations are reported as milligrams of FC-600 per liter 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+1C during this 2-day period (Daily Record of Fish Holding Conditions). The well water which flowed into this tank was characterized as having total hardness and alkalinity ranges as" calcium carbonate (CaCO_) of 250 mg/1 and 230 mg/1, respectively, and a specific conductance ofJ340 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). oozoez 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-j of 250 mg/1 and 230 mg/1, 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/1 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 replacements 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/1 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 andtotal length of 0.42+0.11 grams and 3.8+0.45 cm (Fish Weights and Lengths Log) were randomly distributed to each 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. 0055063 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 material FC-600 was not acutely toxic to fathead minnows at nominal concentrations as high as 1,000 mg/1 (Table 1). No FC-600 related mortality of fish exposed to 1,000 ffig/1 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/1, the highest concentration tested. No control organisms died or showed signs of disease or stress during the test. The temperature in various aquaria ranged from 19-21C during exposure, and did not vary more than 2C 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 and B. J. Halligan. 1978. Manual for construction and operation of toxicity-testing proportional diluters. EPA-600/3-78-072. -- Mount, D. I. and W. A. Brungs. 1967. A simplified dosing apparatus for fish toxicology studies. Water Res. Is 20-29. OECD. 1981. Guidelines for Testing of Chemicals. Organization for Economic Cooperation and Development, Washington, D.C. U.S. EPA. 1982. Environmental Effects Test Guidelines. EPA 560/6- 82- 02* 002064 Table 1 Concentrations tested, corresponding percentage mortalities of fathead minnow (Pimephales promelas) exposed to FC-600 under flow-through conditions. Twenty fish were exposed to each concentration. Nominal Concentration (mg/1) 1000 560 3 20 180 100 Control LC50 (mg/1) - 24 hour Percentage Mortality 48 hour 72 hour $6 hour 00 0 0 00 0 0 00 0 0 00 0 0 0000 0000 >1 ,000 >1,000 >1,000 >1,000 002065 \ "2. *> WELL WATER QUALITY 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 M-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/1 ~ <0.1 mg/1 as N 340 umhos/cm at 25C 230 mg/1 as CaCO^ 280 mg/1 J 250 mg/1 as CaCO- <0.02 mg/1 J <0.4 mg/1 Negative 40 per ml <19 ug/1 1 ug/1 15 ug/1 <5 ug/1 <3 ug/1 <2 ug/1 <0.1 ug/1 11 ug/1 <7 ug/1 <1 ug/1 <5 ug/1 89 ug/1 0.7 ug/1 <0.01 ug/1 <0.01 ug/1 <0.01 ug/1 ENV. LAB WATER QUALITY BOOK RE 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 002066 ENVIRONMENTAL LABORATORY AQUATIC TOXICITY DATA SHEET DEFINITIVE (FULL-SCALE TEST) LR |ryf? i Test^ ^ Tested -flrEr-p- ________ ;t O r g a m s m ^ ^ ^ ^ ^ ^ ^ ^ S o u r c e ^ ^ y ^ \fcR_ Date Rec'd L Z / l f a j Batch # 2 r9^ j.Wt. /jrams Avg. Size ^ B cm No. Orqanisms per dose /^) Loading Factor .g/i ;h Disease Treatment: AMAfF,______________________________________________________ st Solution Volume Cj Liters/All-Glass Tank Tank Dimensions: 35x20 cm and 25 cm deep e Started ^ r Q Q Date Started ______Date Completed ^ / / -ution Water Carbon-filtered well water (Temp, ft C., D.O. fl ppm, pH %.2_} ) ^5 5?-<6nfidence Luivits) ptq/jL - ink Initial Total 24 Hours 48 Hours ~ 72 Hours 96 Hours Cone. Amount Total No. pH D.O. Total No. pH D.O. Total No. pH D.O. Total No. pH D.O. mg/1 Added Dead ppn Dead ppm Dead ppm Dead ppm 0 _ Control CoaIt o I .. <0 7,5 Itti O . 16'14 . O 0 10 O hi lA O Vp b 7 t( |W? O O 16 (p,ci Iff lpt1 1__ LOGO Jl \ttO X ?, ^ L tC>K rest Temp. C Initials & Date TtK^nf-c;* M0 7,7 <5 ~1i(p O .0 7 , 7 Jf<f) O . ~da 0, / O 16k Z - O is (A O (r-l M .. 0 O ^ . 7 , 7 ifPi (& V/2/5C?- 16kZL_ O tiff fa'?) O 1 luc _ j2 _ . Ia I ZDCs 2 flCr\ 11 / r isO if,?, 16(0 b.t , 7-f . ,, :ondary Effects (other than Mortality) : EC50 ENVIRONMENTAL LABORATORY AQUATIC TOXICITY DATA SHEET DEFINITIVE (FULL-SCALE TEST) LR-- fiA * Test^ g < ^ k Y 7 E PjjtorTjfpu$^tezial _______ 5t Orgamsm^ j ^ ^ J cuzce _ 3 $ p M < r' /frfof Date Rec'd u / r j i ^ Batch Z r P ^ j.Wt. 7 , , grams Avg. Size ^ $ cnv No- Organisms per dose / ( ) Loading Factor J 2 M t b g /i sh Disease Treatment: ___________________________ ;t Solution Volume ^ Liters/All-Glass Tank Tank Dimensions: 35x20 an and 25 cm deep Started //;)Q/ ^ / Date Started */////&& Date Conpleted W a y / & ^ -ution Water Carbon-filtered well water (Temp. /(% C., D.O. Q estigator _ __ A.~ k :50 (95% Confidence Limits) ill Si< ppm, pH ) > /rfrt ink Initial Total 24 Hours 48 Hours - 72 Hours 96 Hours 5. Cone. Amount Total NO. pH D.O. Total No. PH D.O. Total No. pH D.O. Total No. pH D.O. mg/ 1 Added Dead ppm Dead ppm Dead ppm Dead ppm 2Jl_ . * 0 . O. 1,(<7 in Ufh O' 0 1U< o n M11a Cj CD M- > ,, < O 1U O f,(f(r,? 1,(c >-3 ! 1! 0 n ?PT> r __ -\0 0 - j tOQXj Test Initials & Date Trvanf-cL- O O O --O 1 1 tl 7,bin, 0 0 O i h O.Zj O 10 (A% n b,1 0 10 mM 7,fe 1 , 1 ki 0 0 u ( ,6) t y^z//j-- J O f.S 0 t i lf<?> n tv 1,0 0 IS (A . z o % \ ' , - Z V -. :ondary Effects (other than Mortality): ink f o . Symptoms or Reactions itrol 24-Hr. EC50 Total Number Affected 48-Hr. 72-Hr. 96-Hr. -- BEST CC 3Y AVAILABLE 1