Document aJrM0dVE41OZNd5aJvQMOmN2e

ACUTE TOXICITY TO FISH (MUMMICHOG) TEST SUBSTANCE Identity:A mixturecontainingperfluorooctanesulfonatmea;y alsobe referredto as PFOS, FC-95,or as a component of FC-203C and L-5440. (1-Octanesulfoniaccid, 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecapfoltuaosrsoi-u,m salt,CAS # 2795-39-3) Remarks: The 3M productionlotnumber was not noted.The test sample isFC-203C and isreferredto by thetestinglaboratoryas "81-1/8". Currentinformatioinndicateistisa mixtureof 1.47% testsubstance,60% water,30% diethyleneglycolbutylether,3% sodium octylsulfate3,% hydroxyfoamer,10% polyoxyethylenemonooctylphenylether,0.12% sodium lauryslulfatea,nd 0.05% benzotriazol. The fbilowingsummary appliesto the testsample as a mixture of the testsubstance in water solutionwith incompletelycharacterized concentradon of impurities.Data may not accurateiyrelatetoxicity of the testsample withthatof thetluorochomicalcomponent METHOD: Method: EG&G, Bionomicsprotocolenfited"ProtocolforFlow-through ToxicitTyestswithFishes,"January,1980. Test type:Flow-throughacute GLP: No Year Completed: 1981 Species:Fundulusheteroclitus Supplier:Commercialsupplier Analyticalmonitoring:Temperature,pH, DO, and salinity Exposure period:96-hours Statisticamlethods: LC50valuescalculateudsingthecomputerprogram (createdby Stephan,1978) based on the moving average angleanalysis (24-,48-,and 72-hourLC5o,s)o,rbinomialprobabilit(y96-hourLC50). Test fishage: Adult. Length and weight: Length = 31 - 37 mm witha mean of35 mm Weight = 0.43 - 0.80g witha mean of0.63g Loading: 0.13 g/L Pretreatment:Not noted. Test conditions: Dilutionwater:Naturalf,ilteresdeawaterfrom Big Lagoon,a Gulf of Mexico estuary,Florida. Dilutionwater chemistry: Salinity: 28 - 29 partsperthousand Lighting:Fluorescentlightpsrovideda dailyphotoperiodof12 hourslight and 12 hours darkwithan intensitoyf 1,100 luxincidentothe water surface. Stock and testsolutionpreparation:A primarystocksolutioonf 523,000 mg/L was preparedby adding 523 grams oftestsample to a 1-L volumetricflaskand bringingto volume withdeionizedwater.AJItest solutionwsere preparedby a dilutedreliverinfgivenominalconcentrations ofthetestsample and controlwater. Flow-through rate:Approximately3 aquariumvolume replacementsper 24 hour period. Stabilitoyfthe testchemicalsolution:Not noted. Exposure vessels:30 x 30 x 91 cm glasstankscontainin-g 50 literosf solutionvolume. Number of replicatest:wo Number of fishper replicate1:0 Number of concentrations:5 plusa blankcontrol Water chemistryduringthe study: pH range (0-96hours): 7.8- 8.0(control) 7.6- 8.0(2000mg/L) Temperature range (0-96hours): 22 - 240C (forallaquaria) Dissolvedoxygen range (0-96hours): 6.3- 7.1mg/L (control) 3.8- 7.1mg/L (2000mg/L) Salinitryange (0-96hours): 28 - 29 partsperthousand(forallaquaria) RESULTS Nominal concentrations:Bk control1,25,250,500, 1000,and 2000 mg/L Percentmortalit(y20fishper concentration) Nominal Concentration (mgfl) Control 125 250 500 1000 2000 24-hours 0 0 0 0 0 90 Percentag mortality 48-hours 72-hours 0 0 0 0 0 0 0 0 0 0 95 95 Whours 0 0 0 0 0 100 Element value: 24-hourLC5o= 1,500(1,400-1,600)mg/L 48-hourLC50= 1,500(1,400-1,600)mg/L 72-hourLC50= 1,500(1,400-1,600)mg/L 96-hourLC5o= 1,400(1,000- 2,000)mg/L Element valuesbased on nominalconcentrations. Remarks: Testingwas conducted on the mixtureofthetestsubstanceas describedinthetestsubstanceremarksfield.The valuereportedapplies tothatmixtureand notthefluorochemicaplroportionalone. CONCLUSIONS The FC-203C 96-hourLC50forFundulus heteroclituwsas determinedto be 1,400 mg/L vatha 95% confidenceintervaolf 1,000to 2,000 mg/L. Submitter:3M Company, EnvironmentalLaboratory,P.O. Box 33331, St. Paul,Minnesota,55133 DATA QUALITY ReliabilityK:Jimischranking2. The studymeets allcriterifaorquality testing.However, sample puritywas notpropedy characterizeadnd the study lacksanalyticaclonfirmatioonftheamount offluorochemical proportioninthe solution. REFERENCES Thisstudywas conducted by EG&G Bionomics Marine Research LaboratoryofPensacola,FL attherequestofthe 3M Company, 3M Lab Request number 7038, 1981. OTHER Last changed: 6/26/00 E,41[# L R "c,.703t Acute toxicity of a surfactant solution (81-1/8) to the mummichog Fandutu,6hetvwctttu,6in a f lowthrough system Toxicity Test Report Submitted to Minnesota Mining & Manufacturing Company Environmental Engineering and Pollution Control Environmental Laboratory St. Paul, Minnesota 55133 Project Number R36 Report Number BP-81-10-163 EG&G Bionomics Marine Research Laboratory 10307 Gulf Beach Highway Pensacola, Florida 32507 October 1981 EG&G Bionomics Marine Research Laboratory 10307 Gulf Beach Highway Pensacola, Florida 32507 TOXICITY TEST SUMIARY SHEET Client: Minnesota Mining and Manufacturing Company Client Contact or Principal Investigator: Mr. Eric Reiner Report date & number: October 1981; BP-81-10-163 Bionomics*. project number: R36 Study Director: Mr. G- Scott Ward Test material: Surfactant solution 81-1/8 Description: Deep orange-yellow liquid Date material received: 12 August 1981 Date of definitive test: 5-9 Octobet 1981 Test condition: Flow-through, 96-hour duration, 231 degrees Celcius Test procedure: BMRL test protocol,"Protocol for Flow-through Tests with Fishes," dated 29 January 1980. Toxicity Test animal: Mummichog; Fundutus heteaoctitus Source and age: Purchased from a.commercial supplier, adults Seawater: Natural, filtered, salinity from Big Lagoon, 28-29 parts per thousand Solvent/carrier: none Nominal test concentrations: ..125, 250, 500, 1,000 and 2,000 milligrams per liter (mg/Y.) Effect criterion: Mortality 96-liour LC50-. 1,400 mg/k 95% confidence limits: 1,000 2,000 mg/t 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 (81-1/8) on the mununichog Fundutu6 heteAoctitu4. The criterion for ef fect was death. Results of the test are reported as 24-, 48-, 72-, and 96-hour LC50 values (the concentrations of test material estimated to be lethal to 50% of the test animals at the specified times of exposure). All data related to this study are stored at BMRL. MATERIALS AND METHODS Test material The test material was received at BMRL on 12 August 1981 in one 9.5 liter (t) cubetainer labeled "3M SAMPLE 81-1/8." The test material, a deep orange-yellow liquid, was tested as received. All test concentrations are reported here as milligrams (ULg)of surfactant solution per i of seawater or as parts per million (ppm). Test animals Mummichogs were purchased from a commercial supplier and maintained at BYIRL in flowing, natural seawater for 5 days. During the 96-hour period immediately before the test, the'salinity of the holding water ivas 28-29 parts per thousand (0/oo) and the temperature was 19-21 degrees Celsius (OC). No mortality was observed during the entire holding period. The control fish were 31-37 millimeters (mm) standard length and 0.43-0.80 grams (g) wet weight; mean length and weight were 35 (S.D.2) rm and 0.63 (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 (um) 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 L/cycle/test aquarium at a dilution rate of 50%. The average number of cycles was approximately 6.4/hour. This cycling rate provided approximately 3.0 volume additions in 24 hours. The surfactant stock solution (523,000 mq/Z) was*prepared by weighing 523 g of surfactant solution in a 1-k volumetric flask and bringing to volume with deionized water. The stock solution was placed in a 4-L glass reservoir attached to a "dipping bird" (Mount and Brungs, 1967). A 14.9 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 volumes of uncontaminated dilution seawater from the water cells with 3 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 50t of test solution or control seawater. Light was provided by two 3.7-m fluorescent bulbs suspended 46 cm above the test containers, providing approximately 1,100 lux incident to the water surface. Photoperiod was 12 hours of light and 12 hours of darkness. Five concentrations of surfactant solution 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 concentration 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. The test was conducted 5-9 October 1981. 4 Statistical analyses Based on the results of the test with the surfactant solution, 24-, 48-, 72-, and 96-hour LC50's and 95% confidence limits were calculated. The computer program estimated LC50 values by three statistical methods; moving average angle.analysis, probit analysis, or binomial probability. The method selected was determined by the characteristics of the data, that is, the presence or absence of 0% and 100% mortality and the number of concentrations in which >0%<100% mortality occurred (Stephan, 1977). The moving average angle method was used to calculate the 24-, 48-, and 72-hour LC50's. The 96-hour LC50 was determined by the bionomial probability method. RESULTS AND DISCUSSION After 24 hours of exposure to the surfactant solution, mortality ranged from 0% in surfactant concentrations <1,000 ppm to 90% in the 2,000 ppm test concentration. The 24 hour LC50 was 1,500 ppm with 95% confidence limits of 1,400-1,600 ppm (Tables 1 and 2). After 96 hours of exposure, mortality of fish ranged from 0% in test concentrations <1,000 ppm to 100% in the 2,000 ppm test concentration (Table 1). The 96-hou-rLC50 was 1,400 ppm with 95% confidence limits of 1,000-2,000 ppm (Table 2). Physical or behavorial abnormalities were observed only in the 2,000- ppm test concentration. After 24 hours of exposure, the 2 surviving fish in 2,000 ppm were observed to be lethargic and remained so until their death. Salinity during the test ranged from 28-29 0/00. The temperature ranged from 22-24OC; mean was 2310C. The dissolved oxygen concentration remained >30% of saturation in all test containers throughout 5 the exposure. The pH was 7.5-8.0 in all test containers throughout the exposure (Appendix A). 6 REFERENCES EG&G Bionomics Marine Research Laboratory. 1980. Protocol for Flow-Through Toxicity Test with Fishes. 2 January 1981. 5 pp. Mount, D.'I. and W. A. Brungs. 1967. A simplified dosing apparatus for fish toxicological studies. Water Research, 1:21-29. Stephan, C.E. 1977. Methods for calculating an LC50. ASTM, Aquatic Toxicology and Hazard Evaluation, ASTM STP 634. P.L. Mayer and J.L. Hamelink, eds. pp. 65-84. 7 TABLE 1. Mortality of mummichogs (Fun&d-" heteAodZW) exposed to a surfactant solution (81-1/8) 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/t;ppm) 24 hour 0 0 0 0 0 90 Mortality 48 hour 72 hour 0 0 0 0 0 0 0 0 0 0 95 95 .96 hour 0 0 0 0 100 8 TABLE 2. Calculated LC50's for mummichogs (Fundut" hetekociu") exposed to a surfactant solution (81-1/8) in flowing natural seawater. Test concentrations are given as nominal concentrations of whole material. Hour 24 48 72 L9 6 LC50 (mgl9.; ppm) 1,500 1,500 1,500 1,400 95% confidence limits (mg/.t;ppm) 1,400-1,600 1,400-1,600 1,400-1,600 1,060-2,OOOJ PREPARED BY: AUDITED BY: 9 G. Scott Ward G. s c.m,-k@ Study Director . 10--&. 2-0 OMCA,@ Date Alan G. Miller Quality Assurance Unit Date Raw data audit: Preliminary report audit: lo' 6e-z@44 Final report audit: ec-lymll Igel REVIEWED AND APPROVED BY: Peter J. shuba, Ph.D. T ordinator Date ri EGZG BIONOMICS Marine Research Laboratory Pensacola, Florida SUBJECT: ACUTE TOXICITY DATA SHEET CLIEW: 3M Carrpany PFDJ= NO: R36 APPENDIX A A-1 PAGE: NO.: BP-QAF-001 EFFECTIVE: December 1980 OPEC IES: Fundulus heteroclitus TEST MATERIAL: Surfactant Solution (8l-v8), ANIMAL HISTORY LOT NO: 9-3c-- gk-A-5*9 SEE PAGE NO: OFI@NIMAL COLLECTIONIRECEIPT LOG FOR RAW DATA DATE MAINTENANCE/ACCLIMATION BEGAN: Tn CONDITION OF ANIMALS: p_x c-P-k @ -441 LIFE STAGE: WRTALITY(%)IN SEE PAGE No. TANK 48 HOURS PRIOR TO TESTING: (1-ri OF FOR RAW DATA TEST CONDITIONS OPRELIMINARY NOEFINITIVE (:]STATIC ZFLOW-TliRU NLLMBER OF ANIMALS/CONTAINER 3, 5,(B 20, TIME ADDED CH&MICAL/ANIMALS %330 NUMBER OF TEST CONTAINERS/CONC 4. TEMPERATURE('C) 20,L22) 30 - TEST SYSTEM OPEN [] CLOSED TEST CHAMBER VOLUME (1) 1, 3.8.19 (.:SF-0i@z.) DILUENT VOLUME (1) 0.9, 3, 15 ik SALINITY (0/oo) AMBIENT PROTOCOL FOLLOWED: CIRCLE ONE: TEST MATERIAL AS ACTIVE INGREDIENT/WHOLE MATERIAL TEST CONCENTRATIONS % mg/l CON- SOLV TROL CONT AMOUNT OF CHEMICAL/STOCK ADDED N.A. N.A. STOCK SOLUTION USED (1*, 2', 3*) A@AOUNT 0.@-SOLI:-@t#ATDDED (rnl) N.A. N.A. tiA.. [ t,-A- N. A. ti.A. tlA.. N.A. ft.A. fl.A. SOLVENT/CARRIER S/C CONCENTRATION ADDITIONAL CO.4,4.ENTS: (DOCUMENT ANY DEVIATIONS FROM PROTOCOL) oc> nZ>EcD-rc3 L310NOfvllCS DATE CONTROL TE14P *C/SAL. T I-YE DATA BY o-iioullt 0 C-'V @ I c O/oo z@ 15 cn!.'CE,'%'TRATION .11/1 REP OBS PH 00 OBS CONTROL 0 B SOLVENT CONTROL A B A I's S,o L.9 24-liOUR 48-HOLIR ci @@:zq O/oo 0/@00 1:33 0 No. DEAD CUM NO DEID CUM DEAD /CC PH DO OBS ID@al ct Ito. 7--T- I -0 o 72-HOUR -I @g Oc c 19 9 t O/oo NO@D/ CDUEMAD OBS PH 00 J.R 6.1 1*'t 6.0 SA ij Ono A 9.o C) A ,-w-eT.g-o 6 rb 1.0 .7.1 A 1 8.01 '7.o B S6 0 A & 7. co> C) o 1-9 a 0 -*.y q.ct S5 0 /0 16 1.9 57, Ea- 0 66 5,6 11' 0 q 0- Ct A B 00 METER USED pH VETER USED t@ L4 SALINI TY lPiEASIJREMEIIT cl@ TEMPERT,TUR@ MEASUREII.Etl TE OBSERVATION KEY NONE OBSERVATION WAS MADE AND NOTHING CUT OF THE ORDINARY WAS OBSERVED AS . [iT THE SURFACE ERR - ERRATIC MSP - l@U4CLE SPASM GY - GYRATING CLE - COt4PLETE LOSS EQUILIBRIUM ORK - DARK PIG@IEIITATION - -'--,AL LOSS EQUILIBRIUM HE.14 . liEMORRMGIC LL.EiTTH - LETH RGIC RA - RAPID RESPIRATION !iyp - HYPERACTIVE G - GULPING CLOY - CLOUDY SOLUTION PRE - PRECIPITATE FOS - FILM ON SURFACE uc - UNDISSOLVED CHEMICAL