Document qkzeJe2bLJQnpb3vgEJnm1aX5

A fi. & Z 6 _ 0 7 t j - 2 A C U T E T O X IC IT Y TO FISH (M U M M ICH O G ) T E S T S U B S T A N C E _____________________________________________ Identity: A mixture containing perfluorooctanesulfonate; may also be referred to as PFO S, FC-95, or as a component of FC-203C and L-5440. (1-Octanesulfonic acid, 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluoro-, potassium salt, C A S # 2795-39-3) Rem arks: The 3M production lot number w as not noted. The test sam ple is FC-203C and is referred to by the testing laboratory a s "81-1/8". Current information indicates it is a mixture of 1.47% test substance, 60% water, 30% diethylene glycol butyl ether, 3 % sodium octyl sulfate, 3 % hydroxy foamer, 10% polyoxyethylene monooctyJphenyl ether, 0.12% sodium lauryl sulfate, and 0.05% benzotriazol. The following summary applies to the test sample as a mixture o f the test substance in water solution with incompletely characterized concentration o f impurities. Data may not accurately relate toxicity o f die test sample with that o f the fluomchemical component M ETH O D:______________________________________________________ M ethod: EG& G, Bionom ics protocol entitled "Protocol for Flow-through Toxicity Tests with Fishes,"January, 1980. T e st type: Flow-through acute GLP: No Y ear Com pleted: 1981 Sp e cie s: Fundulus heteroditus Supplier: Commercial supplier A nalytical m onitoring: Temperature, pH, DO, and salinity E x p o su re period: 96-hours Statistical m ethods: LCso values calculated using the computer program (created by Stephan, 1978) based on the moving average angle analysis (24-, 48-, and 72-hour LCsos). or binomial probability (96-hour LCso)- T e st fish age: Adult. Length and w eight: Length = 3 1 - 3 7 mm with a mean of 35 mm W eight = 0.43 - 0.80 g with a mean of 0.63 g L oad in g: 0.13 g/L Pretreatment: Not noted. T est conditions: Dilution water: Natural, filtered seawater from Big Lagoon, a Gulf of Mexico estuary, Florida. Dilution water chem istry: Salinity: 28 - 29 parts per thousand 001022 Lighting: Fluorescent lights provided a daily photoperiod of 12 hours light and 12 hours dark with an intensity of 1,100 lux incident to the water surface. Sto ck and test solu tion preparation: A primary stock solution of 523,000 mg/L w as prepared by adding 523 gram s of test sam ple to a 1-L volumetric flask and bringing to volume with deionized water. All test solutions were prepared by a diluter delivering five nominal concentrations of the test sample and control water. Flow -through rate: Approximately 3 aquarium volume replacements per 24 hour period. Stability o f the test chem ical solution: Not noted. Exposure v e sse ls: 30 x 30 x 91 cm g la ss tanks containing ~ 50 liters of solution volume. Num ber o f replicates: two Num ber o f fish per replicate: 10 Num ber o f concentrations: 5 plus a blank control W ater chem istry during the study: pH range (0-96 hours): 7.8 - 8.0 (control) 7.6 - 8.0 (2000 mg/L) Tem perature range (0-96 hours): 22 - 24C (for all aquaria) D isso lv e d oxygen range (0-96 hours): 6.3 - 7.1 mg/L (control) 3.8 - 7.1 mg/L (2000 mg/L) Salinity range (0-96 hours): 28 - 29 parts per thousand (for all aquaria) R E S U L T S ____________________________________________ Nom inal concentrations: Bk control, 125, 250, 500,1000, and 2000 mg/L Percent m ortality (20 fish per concentration) Nom inal C o n c e n tra tio n (mg/L) Control 125 250 500 1000 2000 24-hours 0 0 0 0 0 90 P ercen tag e m ortality 48-hours 72-hours 00 00 00 00 00 95 95 96-hours 0 0 0 0 0 100 Elem ent value: 24-hour LC50 = 1,500 (1,400 -1,600) mg/L 48-hour LCso = 1,500 (1,400 -1,600) mg/L 72-hour LC50 = 1,500 (1,400 -1,600) mg/L 96-hour LCso = 1,400 (1 ,0 0 0-2,000) mg/L 001023 Element values based on nominal concentrations. Rem arks: Testing w as conducted on the mixture of the test substance a s described in the test substance remarks field. The value reported applies to that mixture and not the fluorochemical proportion alone. C O N C L U S IO N S ________________________________________________ The FC-203C 96-hour LC 50 for Fundulus heteroclitus w as determined to be 1,400 mg/L with a 9 5 % confidence interval of 1,000 to 2,000 mg/L. Subm itter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 D A T A Q U A LIT Y ________________________________________________ Reliability: Klimisch ranking 2. The study meets all criteria for quality testing. However, sam ple purity w as not properly characterized and the study lacks analytical confirmation of the amount of fluorochemical proportion in the solution. R E F E R E N C E S _____________________________________________ This study w as conducted by EG & G Bionomics Marine Research Laboratory of Pensacola, FL at the request of the 3M Company, 3M Lab Request number 7038, 1981. O T H E R ________ :______________________________________________ L a st changed: 6/26/00 001024 EAI# V i Z l f L R V b. 7 038" Acute toxicity of a surfactant solution (81-1/8) to the mummichog unduZu& hztznjocJUXuJi in a flow through system f 3 C- 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 001025 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: 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 October 1981 Test condition: Flow-through, 96-hour duration, 231 degrees Celcius Test procedure: BMRL test protocol."Protocol for Flow-through Toxicity Tests with Fishes," dated 29 January 1980. Test animal: Mummichog; FunduZuA heXe/LoeZituS Source and age: Purchased from a commercial supplier, adults Seawater: Natural, filtered, from Big Lagoon, 28-29 parts per thousand salinity Solvent/carrier: none Nominal test concentrations: .125, 250, 500, 1,000 and 2,000 milligrams per liter (mg/Jt) Effect criterion: Mortality 9 6 "hour LC50: 1,400 mg/ Z 95% confidence limits: 1,000 - 2,000 mg/ 001026 1 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 mummichog Fimdofod k&teAjocZltuA. The criterion for effect 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 (A) 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 (mg) of surfactant solution per l 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 5 days. During the 96-hour period immediately before the test, the salinity of the holding water was 28-29 parts per thousand (/oo) and the temperature was 19-21 degree Celsius (C). 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 tS.D.2) mm and 0.63 (S.D.0.10) g, respectively. The control fish appeared to be representative of the test population. 001027 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 (vim) 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 2,/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 mg/2,) was prepared by weighing 523 g of surfactant solution in a 1-2, volumetric flask and bringing to volume with deionized water. The stock solution was placed in a 4-2, 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 001028 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 501 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 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. The test was conducted 5-9 October 1981. 001029 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 concentra tion (Table 1). The 96-hour LC50 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 2,00 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 /oo- The temperature ranged from 22-24C; mean was 231C. The dissolved oxygen concentra tion remained >30% of saturation in all test containers throughout 001030 the exposure. The pH was 7.5-8.0 in all test containers throughout the exposure (Appendix A ) . 001031 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, l:21-2g. Stephan, C.E. 1977. Methods for calculating an LC50. ASTM, Aquatic Toxicology and Hazard Evaluation,^ASTM STP 634. F.L. Mayer and J.L. Hamelink, eds. pp. 65-84. 001032 7 TABLE 1. Mortality of mummichogs (Fondofos hz&iocLLtiu>) exposed to a surfactant solution (81-1/8) in flowing natural seawater. Test concentrations are given as nominal concentrations of whole material. Nominal Concentration (mg/.;ppm) Control 125 250 500 1,000 2,000 24 hour 0 0 0 0 0 90 Mortality (%) 48 hour 72 hour 00 00 00 00 00 95 95 96 hour 0 0 0 0 0 100 001033 8 TABLE 2. Calculated LC50's for muitunichogs (FundufoA heXoAocJiUuA J 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 [ 96 LC50 (mg/l ; ppm) 1,500 1,500 1,500 1,400 95% confidence limits (mq/ A ;ppm) 1,400-1,600 1,400-1,600 1,400-1,600 1,000-2,000 / 001034 PREPARED BY: AUDITED BY: G. Scott Ward Study Director 9 Zo Date Alan G. Miller - / ? /? < ? / Quality Assurance Unit Date Raw data audit: /? / Preliminary report audit : / 6 /& / Final report audit: '/9 /9 J / REVIEWED AND APPROVED BY: Peter J. Shuba, Ph.D. a rjJciWw Technical Coordinator Date 001035 B IO N O M IC S Marine Research Laboratory Pensacola, F lo rid a SUBJECT: ACUTE TOXICITY DATA SHEET CLIENT: 3M Company PROJECT NO: R36 APPENDIX A BEST COPY AVAILABLE A-l PAGE: NO.: BP-QAF-001 EFFECTIVE: December 1980 OPECIES: Fundulus heteroclitus TEST MATERIAL: Surfactant Solution (81-1/8 ANIMAL HISTORY LOT NO: q - 3 o - g l - A - S ~ g SEE PAGE NO: OFjANIMAL COLLECTION/REC EIPT LOG FOR RAW DATA DATE MAI NTENANCE/ACCLIMATI ON BEGAN: .<v. ?c _ m i CONDITION OF ANIMALS: g y c eU<>-^____________ '__________ LIFE STAGE: jQ.MORTALITY(X)IN TANK 48 HOURS PRIOR TO TESTING: -- 11/1 SEE PAGE NO. 3 t - -OF t-o b - FOR RAW DATA TEST CONDITIONS PRELIMINARY g| DEFINITIVE Q static ^FLOW-THRU NUMBER OF ANIMALS/CONTAINER 3, 5,(10} 20, - TIME ADDED CHEMICAL/ANIMALS TEMPERATURE(*C) O ^ oo / \3 3 o Z O ,(g ) 30 - NUMBER OF TEST CONTAINERS/CONC TEST CHAMBER VO LU M E/1) 1, 3 .8 , 19 S ' SQ TEST SYSTEM OPEN C L O S E D DILUENT VOLUME (1) 0 .9 , 3 , 15 ( J S > SALINITY (o/oo) AMBIENT PROTOCOL FOLLOWED: Pfo^oc^-A CIRCLE ONE: TEST MATERIAL AS ACTIVE INGREOIENT/WHOLE MATERIAL TEST CONCENTRATIONS % mg/1 vg/l u l/I CON SOLV TROL CONT AMOUNT OF CHEMICAL/STOCK ADDED ( ) N.A. N.A. STOCK SOLUTION USED (1 * . 2 \ 3*) N. A. N.A. T>\ J AMOUNT OF SOLVENT ADDED (ml) N.A. N.A. N.A. N.A. N.A. N.A. N.A. N.A. SOLVENT/CARRIER S/C CONCENTRATION ADDITIONAL COMMENTS: (DOCUMENT ANY DEVIATIONS FROM PROTOCOL) O c k L r W t \ ___________________ S < -JL (-co-__ yl~. SoQ pa A PCs: -*-- ______p ~(rtg.__ tt>--^ __cn.(~ l0 S>.*>, A ____ C /y.r o L -- sL?___ P-C^T-L=-- -<f ^ ___jssva. yg-f c-- JI' "I-.____ S-vje . 1 001036 ^ E G eG bionomics o-hour 24-HOUR 48-HOUR 72-HOUR 96-HOUR f- OATE C ONTROL TEH? 'CiS A L . TIME DATA BY 5o c t s \ 515 C.PC- io-- O s X ^ i n 21 /oo \3HS GrSw I t O c<i. VHSl 133 0 6>5U) 0/00 $ QcV. m i 3 ^ 7 \33o G-^5 ^ Oco\o<r VH9l 24 /oo \33o Ct-.SLP NOMINAL CONCENTRATION @ ) wg / i 5 y l/ 1 CONTROL SOLVENT CONTROL US Z 5o S od l, O 2., O 00 METER USED pH METER L'SEO DO REP OBS pH t a / i ) NO. / NO. DEAD / CUM DEAD / cu m OBS / DE AO pH DO OBS / OEAD pH DO OBS A w o w ir S.o S.oB . w o*j A 3 A % B 66 '~ A ~ SB B SB A >6 B 56 A S B SB A 6& 3 5ft A 9 .0 S .o S.o S.o S.o S .o s.o ^ .0 ?.o % .o B -fri 1 .1 1 .1 O/ O O/ o / .......... u l.S * *7.1 56 o/ o oj 1 .0 1 .1 SB SS O/ o 0 /. Q U 1 .1 7 .0 1 .0 l. o f S6 54 ib St> UM n .T o o /o o/o D /o /a 7,1 A / / * *1 T *.1 rfO-df O / O /i-0 ^ 4 ^ O Z jP 7-- A U .T- /06^< S . ? ( i -- SB ---- s6 /_ O 7T T-.'T U . O S A o ,o o / o /o $A -- 5ft -- - 56 S- / o oS',4 / O -- -- SB -- -- 56 5 > L t c t H o / 0 /o oA _ T -1 H-Vo S I / 1 H . 56 SH - s& -- - s& 3 - 'i f * S .f / J 4 rq NO. DEAD /' cu m DEAD pH DO OBS 0 / 'o o T -A M - NOV^ I rJOJf / V / T -f O/ o 0 /o . ' / ' 0/ /o 0 / 'o -- >? -- -- SB 5b -- Sb -- S6 Sm s . t JA -- 52, -- S6 O /} H \ S.ia ---- / NO. DEAD / CUM / DEAD pH 00 o /Q 3-. 3 L ..3 0 T - ? < - rs / o IT o /o o /o o/o oA _ /o c o/ o \/ o / lo T-.Ts.s H .? S*.o 7-T- H u T .T - H u 3. S ' 3 .*r 2 .\ p L k ^ 3.<P -- / *\ tL ^ S A L IN IT Y MEASUREMENT TEMPERATURE MEASUREMENT S c .t -^1 Sc,"r*| SCX * _____StT *A _ OBSERVATION KEY NONE - O BSERVATIO N WAS MADE AND NOTHING OUT OF THE ORDINARY WAS OBSERVED AS - AT THE SURFACE ERR - ERRATIC MSP - MUSCLE SPASM i GY - GYRATING CLE - COMPLETE LOSS EQ U ILIBR IU M ORK - DARK PIG MENTATIO N PLE - PARTIAL LOSS EQ UILIBRIU M HEM - HEMORRHAGIC LETH - LETHARGIC RA - RA PID RESPIRATION HYP - H YPERACTIVE G - GULPING S c T "``l s c.r M S& - CLOY PRE FOS UC S o PiP - U . E G O B B L E S *T>ie s o t p iv c e - CLOUDY SOLUTION - PRECIPITATE - F IL M ON SURFACE - UNDISSOLVEO CHEMICAL / ---- ------- ------ ---- Scr Ser* l S ^ x cT^\ TEST KEY BEST COPY AVAILABLE >I N>