Document v2pX5BNdKBap1YjvRG6KVv7R

A R .& & 6 _ O S O H - A C U T E T O X IC IT Y TO F IS H (M U M M IC H O G ) T E S T S U B S T A N C E ____________________________________________________ Id en tity: A mixture containing perfluorooctanesulfonate; m ay also be referred to as P F O S , FC-95, or as a com ponent of FC-206C and 81-2/8. (1-O ctanesulfonicadd, 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) R em arks: The 3M production lot number w as not noted. The test sam ple is FC-206C and is referred to by the testing laboratory as "81-2/8". Current information indicates it is a mixture of 0.73% P F O S , 76.09% w ater, 15% diethylene glycol butyl ether, 4 % urea, 1,55% sodium octyl sulfate, 1.47% hydroxy foam er, 1.05% polyoxyethylene m onooctylphenyl ether, 0.06% sodium lauryl sulfate, and 0.05% benzotriazole. The following summary applies to a mixture with incompletely characterized concentration o f impurities. Data may not accurately reflect the toxicity o f the fluorochemical compnent o f the test sample. M ETH O D :_________________________________________________________________ M ethod: EG & G , Bionom ics protocol entitled "Protocol for Flow-through Toxicity Tests with Fish es," Jan u ary 2,1980. T e st typ e: Flow-through acute G L P : No Y e a r C om pleted: 1981 S p e c ie s : Fundulus heteroclitus S u p p lie r: Com m ercial supplier A n a lytica l m onitoring: Tem perature, pH, DO, and salinity Ex p o su re p erio d : 96-hours S ta tis tic a l m ethods: LC 50 valu es could not be calculated. T e st fish ag e: Ju ven ile. Leng th and w eig h t: Length = 2 7 - 3 5 mm with a m ean of 31 mm W eight = 0.28 - 0.63 g with a m ean of 0.46 g Lo ad in g : 0.092 g/L Pretreatm en t: Not noted. T e st co n d itio n s: D ilutio n w ater: Natural, filtered seaw ater from Big Lagoon, a G ulf of Mexico estuary, FL. D ilutio n w a te r ch em istry: S a lin ity : 27 -28 parts per thousand 001672 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 w ater surface. Stock and test solution preparation: A primary stock solution of 502,000 mg/L w as prepared by adding 502 gram s of test sam ple to a 1-L volum etric flask and bringing to volum e with deionized w ater. All test solutions w ere prepared by a diluter delivering five nominal concentrations of the test sam ple and control w ater. Flow-through rate: Approxim ately 1.5 aquarium volum e replacem ents per 24 hours. Stability of the test chemical solution: Not noted. Exposure vessels: 30 x 30 x 91 cm glass tanks containing ~50 L of test solution volum e. Number of replicates: two Number of fish per replicate: 10 . .. Number of concentrations: 5 plus a blank control Water chemistry during the study: pH range (0-96 hours): 7.8 - 7.9 (control exposure) 7.4 - 8.0 (2000 mg/L exposure) Temperature range (0-96 hours): 22 - 2 7 C (for all aquaria) Dissolved oxygen range (0-96 hours): 5.7 - 6.9 mg/L (control exposure) 0.6 - 6.8 mg/L (2000 mg/L exposure) Salinity range (0-96 hours): 27 - 28 parts per thousand (for all aquaria) Remarks: During the third day of exposure, the diluter stopped cycling and resulted in only 6 cycles (1 L solution / cycle) for the 24 hour period. Sin ce the test concentration did not change, it w as concluded that this did not affect the validity of the test. R E S U L T S _________________________________________________________________ Nominal concentrations: Bk control, 125, 250, 500,1000, and 2000 mg/L Element value: 24-hour LC 50: 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 Elem ent valu es based on nominal concentrations. Remarks: Testing w as conducted on the mixture as described in the test substance rem arks field. The value reported applies to that mixture and not the fluorochem ical proportion alone. 001673 C O N C LU SIO N S The FC-206C 96-hour LC 50 for Fundulus heteroclitus w as determ ined to be >2,000 mg/L, the highest concentration tested. 10% m ortality w as observed at this concentration. S u b m itte r 3M Com pany, Environm ental Laboratory, P.O . Box 33331, St. Paul, M innesota, 55133 D ATA Q U A LIT Y ___________________________________________________________ R e lia b ility : Klim isch ranking 2. The study m eets all criteria for quality testing. However, sam ple purity w as not properly characterized and the study lacks analytical confirm ation of the am ountof fluorochem ical proportion in the solution. Additionally, D.O. concentrations fell significantly below acceptable levels. R E F E R E N C E S ____________________________________________________________ This study w as conducted by EG & G , Bionom ics of Pensacola, F L at the request of the 3M Com pany, 3M Lab Request number 7038,1981. O T H ER __________________________________________________________________ L a s t ch an g ed : 6/26/00 001674  A Z & P-iZiP C f r 705 r Acute toxicity of a surfactant solution to the mummichog (Fundulus heteroclitus) in a flow-through system ^-z_/r F C - 2 o C. Toxicity Test ReportSubmitted 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 for Flow-Through Toxicity Tests with Fishes" ' 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, and 2,000 milligrams ' (mg)/liter (Ji) . \ Effect criterion: Mortality 96-hour LC50: Could not be calculated; maximum mortality was 10% in 2,000 mg/i. 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 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. MATERIALS AND METHODS Test material The test material was received at BMRL on 12 August 1981 in one 9.5-liter () cubetainer labeled 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 of seawater, or as parts per million (ppm) . Test animals Mummichogs were purchased from a commercial supplier and maintainec 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 (/oo) and the temperature was 21-22 degrees Celsius (C) . 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.iO.lO) g, respectively. The control fish appeared to be representative of the test population. 0 0 i 6 ^ ' ' v| 2 Test water Water used to maintain and test the fish was natural seawater whicl 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 t- ' through hard polyvinylchloride (PVC) pipes, through sand-filled ' fiberglass filters, through charcoal-filled fiberglass filters, and through 10-micrometers (ym) 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 /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 approxiraatel; 1,,5 volume additions in 24 hours. .- ^ The surfactant stock solution (502,000 mg/%) was prepared by weighing 502 g of surfactant solution in a 1-i, volumetric flask and bringing to volume with deionized water. The stock solution was placed in a 4-i, 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 % of . ** s ' test solution of 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 stoppe< 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 surfactarft 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 only 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 fish was apparonfiy dfu-fr0-" than normal. 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 mnnpnt-rat-i nns . Mean salinity during the test ranged from 27-28 /oo* The temperature ranged from 22-27C; mean was 252C. 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 dav 3. The pH was 7.4-8.0 in all test containers throughout the exposure (Appendix A ) . 0016SQ, REFERENCES EG&G Bionomics Marine Research Laboratory. 1980. Protocol for 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 (mg/i ;ppm) Control 125 250 500 1,000 2,000 . __________ Mortality (%) 24 hou r 48 hour 72 hour 000 00o 0 0. 0 000 000 000 96 houj 0 0 o 0 0 <s> 0 0 1 .6 8 2 PREPARED BY: G. Scott Ward Study Director 7 Date AUDITED BY: Alan G. Miller *1 Quality Assurance Uriit ' Raw data audit: Preliminary report audit: Final report audit: m Date REVIEWED AND APPROVED BY: Peter J. Shuba, Ph.D. Technical Coordinator Date 0016S3 J^ E G z G BIONOM ICS Marine Research Laboratory Pensacola, F lo rid a SUBJECT: ACUTE TOXICITY DATA SHEET C L IE N T : 3M C o m p an y PROJECT N O :R 3 6 APPENDIX A A-I PAGE: H O .i BP-QAF-001 EFFEC TIVE: December 1980 S P E C IE S : F u n d u lu s h e t e r o c lit u s : TEST MATERIAL: S u r f a c t a n t s o l u t i o n j ANIMAL HISTORY LOT NO W ___________OF4 ANIMAL COLLECTION/RECEIPT LOG FOR RAH DATA 4 DATE MAINTENANCE/ACCLIMATION BEGAN: C0N0ITI0N OF ANIMALS: L IF E STAGE: MORTALITY(X)IN TANK 48 HOURS PRIOR TO TESTING: lW -- o SEE PAGE NO. O I OF VVoUntOt t-c-O- FOR RAW DATA TEST CONDITIONS pr elim in a r y ^ D EFIN IT IV E sta tic INFLOW-THRU TIME ADDED CHEMICAL/ANIMALS / 5 3 0 TEMPERATURE(*C) 2 0 ,(2 2 ) 30 - TEST SYSTEM OPEN g CLOSED NUMBER OF ANIMALS/CONTAINER 3, 5, (fo j 20, - NUMBER OF TEST CONTAINERS/CONC 1 , 4 , - TEST CHAMBER VOLUME (1 ) 1 ,3 .8 ,1 9 fa ) DILUENT VOLUME (1 ) 0 .9 , 3, 15 SALINITY (/oo) AMBIENT u r r " PROTOCOL FOLLOWED: kc^PA- C Pro Co\ / . *t ubC . ^ CIRCLE ONE: TEST MATERIAL AS ACTIVE INGREDIENT/WHOLE MATERIAL TEST CONCENTRATIONS X mg/1 ug/1 ul/1 (AMOUNT OF CHEMICAL/STOCK ADDED - ) ' CON SOLV TROL CONT N.A. N.A. STOCK SOLUTION USED (1 * . 2 *. 3 ') N.A. N.A. \A \ tt AMOUNT OF SOLVENT ADDED (m l) K>&N.A. N.A. N.A. N.A. N.A. N.A. N.A. N.A. N.A. SOLVENT/CARRIER D& tbniY^. . VGoVe<- S/C CONCENTRATION /OR ADDITIONAL COMMENTS: (DOCUMENT ANY DEVIATIONS FROM PROTOCOL) 001684 1 ^G zE B IO N O M IC S O-HOUR J 24-HOUR 43-HOUR 72-HOUR 96-HOUR DATE CONTROL TEMP *C/SAL. TIME DATA BY NOMINAL CONCENTRATION (nig/Vyiig/1 % u l/l REP ScA-YTSv )!SP?i A ^ < ^ S C ^3--- C^?7o \5cio /S2f GCv^s^civu 1 /fer1 f C/fe- NO. / DO I /DEAD CUM ) JOBS pH- {mg/1 OBS / DEAO pH DO OBS /Z 5 ^ / V/ /S S e ^ / <?/ H sePsi //s/y-0/00 Z-Sr't / /oo /T/" 15oo /?S^n WM- NO. / NO. / NO. / DEAD /CUM DEAD /CUM /DEAD CUM / DEAD pH DO OBS / DEAD pH DO OBS / DEAD PH DO CONTROL A b ! Iw"* o / 7.9 61 /VM' o / o 7* S.9 / 7 * 5,7 floioe o / o B o j o 7.9.2 ' 0 / 0 7.9 5 7 tOdv-tr / 7 * S ? fJO& o / o SOLVENT CONTROL \xr aro A // B A S T-fl /, iW / Uf o 7 a 7? SA ioii O / o B S -1 U.f 5? o / o 7 t S.2 50 o / p A SO TT (.ff Si o / o -- 5*6 o f o B SO S.o fe-K 6- .o / o __ -- -- sa o / o / -`r)nA / 7 7 & 3 f^1 o / o 77 /o - - S / o -- -- s / / 7 5 J.S c4l6OY o / o 3.S CA-OV 46 o /o --- -OY Sfc o /o -- txoY Sft .P /o 5oo A S T-`1 B SG S\0 o /o o /o 7-S 9.5 s o / e > ?Z z? S|? /o 7 ^ // ml sh /o 7.S o / o 7-6 5.s o / o 7.57 ? M6-8O>S . o / o Vjo o o A S I..T- S3 O / 0 B R.o to.)? S* o / d 56 / o -- -- S6 o / o -- -- 56 - - 56 &/z> o/o c/tor -- s?) / o -- DSCfOtY / o A S (a.R a , o o o ______ B SQ *.o U.3 o/o V -1 5 6 o / o__ 7.5 /V ?$> o / o o / o l i l 5 & < 0 / 0 7.5 /3 $ s o / o 7 / 6,iOf. 7.9 <p^ <LU>i W 3./A A 1: / / / / B 1' / / - z. DO METER USED *L ^/ 7/ */ pH METER USED d? SALINITY MEASUREMENT S2ZL $c,r*/ scr^-/ JM?L SoT *' TEMPERATURE MEASUREMENT -ilinli </*- 1 sc.r^i &TH SCT^I 71 71 6.5 71 57 71 i 71 Vit 31 71 3.3 7. 5 1 71 31 7.i 31 7 ? V,/ 7 1 4*7 OBSERVATION KEY TEST KEY NONE - OBSERVATION WAS MADE AND NOTHING OUT OF THE' ORDINARY WAS OBSERVED A5 - AT THE SURFACE, ERR - ERRATIC MSP - MUSCLE SPASM ! GY - GYRATING ' CLE - COMPLETE LOSS EQUILIBRIUM ORK - DARK PIGMENTATION PLE - PARTIAL LOSS EQUILIBRIUM HEM - HEMORRHAGIC LETH - LETHARGIC RA - RAPID RESPIRATION HYP - HYPERACTIVE G GULPING CLDY - CLOUDY SOLUTION PRE - PRECIPITATE FOS - FILM ON SURFACE uc - UNDISSOLVED CHEMICAL *s - *\<1/ ' A l f i V i BEST COPY AVAILABLE ---- >I to 001685