Document gD0Q7LgQ43nz19rea1qZ8g7nV

ACUTE TOXICITY TO FISH (MUMMICHOG) TEST SUBSTANCE Identity:A mixturecontainingperfluorooctanesulfonatmea;y alsobe referredtoas PFOS, FC-95, oras a component ofFC-206C and 81-2/8.(1-Octanesulfoniaccid, 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafploutoarsos-i,um salt,CAS # 2795-39-3) Remarks: The 3M productionlotnumber was notnoted. The test sample isFC-206C and isreferredtoby thetestinglaboratoryas "81-2/8". Currentinformationindicatesitisa mixtureof0.73% PFOS, 76.09% water,15% diethyleneglycolbutylether,4% urea,1.55% sodium octyl sulfate,1.47% hydroxyfoamer, 1.05% polyoxyethylenemonooctylphenyl ether,0.06% sodium laurylsulfatea,nd 0.05% benzotriazole. The followingsummary applies toa mixture with incompletely characterizedconcentration of impurities.Data may not accurately mflect the toxicityof the fluorochemical compnent of the test sample. METHOD: Method: EG&G, Bionomics protocolentged "ProtocolforFlow-through ToxicityTestswithFishes,"January 2, 1980. Test type: Flow-throughacute GLP: No Year Completed: 1981 Species:Fundulusheteroclitus Supplier:Commercial supplier Analyticalmonitoring:Temperature,pH, DO, and salinity Exposure period:96-hours Statisticamlethods: LC50 valuescouldnotbe calculated. Test fishage: Juvenile. Length and weight: Length= 27 - 35 mm witha mean of31 mm Loading: 0.092g/L Weight = 0.28 - 0.63g witha mean of0.46g Pretreatment:Not noted. Test conditions: Dilutionwater:Naturalf,ilterseedawaterfromBigLagoon,a Gulf ofMexico estuary,FL. Dilutionwater chemistry: Salinity: 27 -28 partsperthousand LightingF:luorescelnitghtpsrovideaddailpyhotoperiofd12hourslight and 12 hours darkwithan intensitoyf 1,100 luxincidentothe water surface. Stock and testsolutionpreparation: A primarystocksolutionof 502,000 mg/L was prepared by adding 502 grams oftestsample toa 1-L volumetricflaskand bringingtovolume withdeionizedwater. Alltest solutionswere preparedby a dilutedrelivedngfivenominal concentrations ofthetestsample and controlwater. Flow-through rate:Approximately1.5aquadum volume replacements per 24 hours. Stabilityof the testchemical solution:Not noted. Exposure vessels:30 x 30 x 91 cm glasstankscontaining-50 L oftest solutionvolume. Number of replicates:two Number of fishper replicate:10 Number of concentrations: 5 plusa blankcontrol Water chemistry during the study: pH range (0-96hours): 7.8- 7.9(controlexposure) 7.4- 8.0(2000 mg/L exposure) Temperature range (0-96hours): 22 - 27'C (forallaquaria) Dissolved oxygen range (0-96hours): 5.7- 6.9 mg/L (controelxposure) 0.6- 6.8mg/L (2000 mg/L exposure) Salinityrange (0-96hours): 27 - 28 partsperthousand (forallaquaria) Remarks: Duringthethirdday ofexposure,the dilutesrtopped cycling and resultedinonly6 cycles(1 L solutio/ncycle)forthe24 hour period. Since thetestconcentrationdidnotchange, itwas concluded thatthisdid notaffecthe validitoyfthetest. RESULTS Nominal concentrations: Bk control,125, 250, 500, 1000, and 2000 mg/L Element value: 24-hour LC50: 48-hour LC50: 72-hour LC50: 96-hour LC50: >2,000 mg/L >2,000 mg/L >2,000 mg/L >2,000 mg/L Element valuesbased on nominalconcentrations. Remarks: Tesbng was conducted on the mixtureas descdbed inthe test substance remarks field.The valuereportedappliestothatmixtureand notthe fluorochemicalproportionalone. CONCLUSIONS The FC-206C 96-hour LC50forFundulus heteroclituwsas determined to be >2,000 mg/L, thehighestconcentratiotnested.10% mortalitwyas observed atthisconcentration. Submifter: 3M Company, EnvironmentalLaboratory,P.O. Box 33331, St. Paul,Minnesota,55133 DATA QUALITY ReliabilityK:limischranking2. The studymeets allcriterifaorquality testing.However, sample puritywas not propedy charactenzedand the studylacksanalyticaclonfirmationoftheamount offluorochemical proportioninthesolution.AdditionallyD,.O. concentrationfsell significantbleylow acceptablelevels. REFERENCES This studywas conducted by EG&G, Bionomics ofPensacola,FL atthe requestofthe 3M Company, 3M Lab Request number 7038, 1981. OTHER Last changed: 6/26/00 E,41 7o3 p- Acute toxicity of a surfactant solution to the mummichog (Fundulus heteroclitus) in a flow-through system FC--206 Toxicity Test Report Submitted to Minnesota Mining & Manufacturing Co. Environmental Engineering and Pollution Control Environmental Laboratory St. Paul, Minnesota 55133 Project'Number R36 Report Number BP-81-9-151 EG&G Bionomics marine Research Laboratory 10307 Gulf Beach Highway Pensacola, Florida 32507 September 1981 EG&G Bionomics Marine Research Laboratory 10307 Gulf Beach Highway Pensacola, Florida 32507 TOXICITY TEST SUMMARY SHEET Client: Minnesota Mining and Manufacturing Company Client Contact or Principal Investigator: Dr.* Eric Reiner Report date & number: September 1981; BP-81-9-151 Bionomics project number: R36. Study Director: Mr. Scott Ward Test material: Surfactant solution, 20% butyl carbitol Description: Deep orange-yellow liquid Date material received: 12 August 1981 Date of definitive test: .10-14 September 1981 Test condition: Flow-through, 96-hour duration Test procedure: BMRL's Test Protocol: "Protocol Toxicity Tests with Fishes" for Vlow-Through Test animal: mummichog, Fundulus heteroclitus Source and age: Commercial supplier, juveniles Seawater: Natural, filtered, 27-28 parts per thousand salinity Solvent/carrier: None Nominal test concentrations:--125,@250,-,500,.1,000,. (mg)/liter (t) Effect criterion. Mortality and 2,.000 milligrams 96-hour LC50: Could not be calculated; 2,000 mg/t maximum mortality was' 10% in A flow-through marine toxicity test was conducted at EG&G Bionomics Marine Research Laboratory (BMRL), Pensacola, Florida, to determine the acute effect of a surfactant solution on the mummichog (Fundulus heteroclitus). The criterion for effect was death. Results of the test are reported as a 96-hour LC50 value (the concentration,of test. material estimated to be lethal to 50% of the test animals after 96 hours of exposure). All data related to this study are stored at BMRL. Test material MATERIALS AND METHODS The test material was recei BMRL on 12 August 1981 in one 9.5-liter (Z) cubetainer labeled 3M SAMPLE 81-2/8." I,. A deep orange-yellow liquid, was -tested as receivec. The test material, All test concentrations are reported here as milligrams (mg) of surfactant solution per t of seawater.or as parts per million (ppm). Test animals Mummichogs were purchased from a commercial supplier and maintained at BMRL in flowing, natural seawater for 15 days. During the 96-hour period immediately before the test, the salinity of the holding water was 27-28 parts per thousand (0/oo) and thetemperature was 21-22 degrees Celsius (OC). No mortality was observed during the entire holding period. The control fish were 27-35 millimeters -(mm) standard length and 0.28-0.63 grams (g) wet weight; mean length and weight were 31 (S.D.2) mm and 0.46 (S.D.0.10) g, respectively. The control fish appeared to be representative of the test population. 2 Test water Water used to maintain and test the fish was natural seawater which was pumped from Big Lagoon, a Gulf of Mexico estuary adjacent to BMRL. The pump intake was located about 80 meters (m) offshore at a depth of approximately 3 m. Water was pumped by a 316 stainless steel pump through hard polyvinylchloride (PVC) pipes, through sand-filled fiberglass filters, through charcoal-filled fiberglass filters, and through 10-micrometers (pm) pore size polypropylene core filters into an elevated fiberglass reservoir. Water was chilled by Teflon@ heat exchangers and flowed by gravity into the laboratory. Test conditions Methods for the 96-hour flow-through test were those described in BMRL's "Protocol for flow-through toxicity tests with fishes" dated 2 January 1980. The test was conducted in an intermittent-flow system by using a proportional diluter (Mount and Brungs, 1967) constructed to deliver 1 Z/cycle/test aquarium at a dilution rate of 50%. The number of cycles was approximately 3.2/hour, except during day 3 when the diluter cycled only 6 times in 24 hours because of a malfunction. The cycling..rate of 3.2 cycles/hour provided-approximately 1-5 volume additions in 24 hours. The surfactant stock solution (502,000 mg/k) was prepared by weighing 502 g of surfactant solution in a 1-t volumetric flask and bringing to volume with deionized water. The stock solution was placed in a 4-t glass reservoir attached to a "dipping bird" (Mount and Brungs, 1967). A 15.5 milliliter volume of stock solution was delivered into the mixing cell via the dipping bird during each diluter cycle. A Teflon solenoid valve, controlled by float switches, regulated seawater flow into the water cells. Mixing of various 3 volumes of uncontaminated dilution seawater from the water cells with various volumes of stock solution in the test material cells produced the five concentrations of test material which were distributed to the appropriate test chambers. Test chambers were 30 centimeters (cm) x 30-cm x 91-cm glass aquaria which contained approximately 50 k of test solution or control seawater. Light was provided by two 3.7-m fluorescent blubs suspended 46 cm above the test containers, providing approximately 1100 lux incident to the water surface. Photoperiod was 12 hours of light and 12 hours of darkness. Five concentrations of surfactant solution and and a control were maintained.. Selection of surfactant solution concentrations were based on the results of a 96-hour static test and a maximum test concentra- tion established by verbal authorization from Mr. Eric Reiner of the 3M Company. The nominal concentrations were 125, 250, 500, 1,000, and 2,000 ppm. To begin the test', the diluter cycled until all test chambers were filled with test solutions or control seawater. Ten fish were then placed into each duplicate test container. Survival of fish in all treatments was recorded at 24-hour intervals. The dissolved oxygen concentration and pH were measured in each test container at 0 and 96 hours and in both controls, low, middle, and high test solutions after 24, 48, and 72 hours of exposure. The temperature and salinity were measured in both controls daily throughout the test. Diluter function was checked daily by observation. Only one problem occurred. During the third day of exposure the diluter stopped cycling shortly after the test was checked on a weekend. This problem, 4 however, did not result in any change in the test concentrations and therefore did not affect the validity of the test. The test was conducted 10-14 September 1981. RESULTS AND DISCUSSION After 96 hours of exposure to surfactarlt solutions, mortality of fish ranged from 0% in test concentrations <1,000 ppm to 10% in the 2,000 ppm test concentration (Table 1). A 96-hour LC50 could not be calculated because mortality in the maximum test concentration was <50%. Physical or behavioral abnormalities were observed Qnly in the 2,000 ppm test concentration. After 24 hours of exposure, 4 fish were observed to be darker than normal, however, this was observed again only after 96 hours when 1-fi-sh was--a @Mn n@ormal. After 72 hours of exposure, 11 fish were observed at the surface of the water in the 2,000 ppm test concentration. This probably occurred because of the diluter malfunction and correspondingly low dissolved oxygen concentrat"l nrt-c;. Mean salinity during the test ranged from 27-28 O/oo. The temperature ranged from 22-27OC; mean was 2520C. The dissolved oxygen concentration remained >9% of.saturation in all test containers through- out the exposure. Dissolved oxygen concentrations were low after 48 and 72 hours of exposure, especially in the 2,000 ppm test concentration. The low DO may have been caused by a high oxygen demand after 48 hours and the lack of changeover during day 3. The pH was 7.4-8.0 in all test containers throughout the exposure (Appendix A). 5 REFERENCES EG&G Bionomics Marine Research Laboratory. 1960. Protocol for 1 Flow-Through Toxicity Tests with Fishes. 2 January 1981. 5 pp- Mount, D.I. and W.A. Brings. 1967. A,simplified dosing apparatus for fish toxicological studies. Water Research, 1:21-20. 6 TABLE 1. Mortality of mummichogs (Fundulus heteroclitus) exposed to a surfactant solution in flowing natural seawater. *Test concentrations are given as nominal concentrations of whole material. Nominal Concentration Control 125 250 500 1,000 2 000 (mg/k;ppm) 24 hour 0 0 0 0 0 0 Mortality 48 hour 72 hour 0 0 0 0 0 0 0 0 0 0 0 0 96 hour 0 0 0 0 0 PREPARED BY: G. Scott Ward G. Study Director 7 ]5ate AUDITED BY: Alan G. Miller Quality Assurance Urfit Ljcxr-e /.ofa44 /Y.P/ Raw data audit: I Preliminary report audit: lg"f,@&419pl IF Final report audit: REVIEWED AND APPROVED BY: Peter J. Shuba, Ph.D. Technical Cbordinator Date p IZZEYGiz G BIONOMICS Marine Research Laboratory Pensacola, Florida SUBJECT: ACUTE TOXICITY DATA SHEET CLIENT: 3M Company pRW= NO: R 36 APPENDIX A A-1 PAGE: NO.z BP-QAF-001 EFFECTIVE: December 1980 SPECIES: -TEST MATERIAL: Fundulus heteroclitus Surfactant solution ANIMAL HISTORY LOT NO: 2-k, - o, (I- cj SEE PAGE NO: COLLECTION/RECEIPT 11;131 ()F4ANIMAL LOG FOR RAW DATA DATE MAINTENANCE/ACCLIMATION CONDITION OF ANIMALS: LIFE STAGE: BEGAN: ;7-& AOC"? I fF)L,-C--kte.,+ 3 MORTAL M (%)IN TATIK 48 HOURS PRIOR TO TESTING: % iqti Ft5iA SEE PAGE NO. OF "LibktOC. Lt6C- FOR RAW DATA TEST CONDITIONS PRELIMINARY 1% DEFINITIVE [:]STATIC MFLOW-THRU NU.MBER OF ANIMALS/CONTAINER 3, 5,(920, - TIME ADDED CHFMICAL/ANIMALS 15,3c> TEMPERATURE(-C) 20,030- NUMBER OF TEST CONTAINERS/CGNC I,f,"4*,i- TEST CHAMBER VOLUME (1) 1, 3.8, 19 TEST SYSTEM OPEN CLOSED DILUENT VOLUME (1) 0.9, 3, 15 - SAL IN ITY (D/oo) AM91ENT_le,- PROTOCOL FOLLOWED: CIRCLE ONE: TEST MATERIAL AS ACTIVE INGREDIENT/WHOLE MATERIAL TEST CONCENTRATIONS % mg/i ug/l til/I CON- SOLV TROL CONT AMOUNT OF CHEMICAL/STOCK ADDED N.A. N.A. STOCK SOLUTION USED (1', 2*, 3') N.A. N.A. AMOUNT OF SOLVENT ADDED (ml) ti.A. l@)AIN.A. N.A. N.A.1 14. ADDIT10NAL COMMENTS: (DOCUMENT ANY DEVIATIONS FROM PROTOCOL) SOLVENT/CARRIER D N.A. N.A. N.A. S/C CONCENTRATION A) PI 2_0--CHHOIURUCR,A 24-HOUR 8-ilouR DATE COP@TROL TE@IP 'C/SAL. TIME U/oo c 2(- c 0 /00 DATA BY NO.MI!IAL CONCE:;TRATION (Eg /-@, i!g/l% ill/I REP OBS -1- NO. D0mg7/1) DEAD CUM PH @Bs DEAD - - /D C OBS 11 1 10 1 NO. DEAD CUM DTE DEUAMADD PH CONTROL -I.q U.q AJDKZ'_ 7,9 (,.1IVIIIY%14 00 OBS SOLVEt4T A COTITROL B C.2 o/o 7.9 A '77 7.7 A e-) - -sS. 0 5c3 0 A 0/0 6"'6 t e c> J2 C> A IS13 -@ql(:) - - oc-o B L A*A It G. 9- ? 1. 67 B tAA8 @.-5- L 72-HOUR c O/oo DEA CUM DEAD 6 00 DO77 00 75, CL(IL '38 UA)i ;7 Dr i@) Di@O C) DOMETER USED PH METER USED SALINITY MEASUREMENT T EIIPERATURE MEASUREMENT OBSERVATION KEY NONE - OBSERVATION WAS MADE AND NOTHING OUT OF THE'ORDINARY WAS OBSERVED AS - AT THE SURFACE ERR - ERRATIC MSP - MUSCLE SPASM GY - GYRATING CLE - COMPLETE LOSS EQUILIBRIUM DRK ' - DARK PIGMENTATION PLE - PARTIAL LOSS EQUILIBRIUM HEM - tiEt4URRKAGIC LETH - LETHARGIC RA - RAPID RESPIRATION IHYP - HYPERACTIVE G - GULPING CLOY - CLOUDY SOLUTION PRE - PRECIPITATE FOS - FILM ON SURFACE UC UNDISSOLVED CHEMICAL :!4z rol TEST KEY one,