Document MMDZ2D1Qd2xL036L16V6bdE17

: ARRRE -- OJ0H ACUTE TOXICITY TO FISH (MUMMICHOG) TEST SUBSTANCE Identity: A mixture containing perfluorooctanesulfonate; may also be referred to as PFOS, FC-95, or as a component of FC-206C and 81-2/8. (1-Octanesulfonic acid, 1,1.2,2,3,3,4,4,5,56,6,7,7,8,8,8-heptadecafluoro-, potassium salt, CAS # 2795-39-3) Remarks: The 3M production lot number was not noted. The test sample is FC-206C and is referred to by the testing laboratory as "81-2/8". Current information indicates it is a mixtureof 0.73% PFOS, 76.09% water, 15% diethylene glycol butyl ether, 4% urea, 1.55% sodium octyl sulfate, 1.47% hydroxy foamer, 1.05% polyoxyethylene monooctylphenyl ether, 0.06% sodium lauryl sulfate, and 0.05% benzotriazole. The following summary applies to a mixture with incompletely characterized concentration of impurities. Data may not accurately reflect the toxicityofthe fluorochemical compnentofthe test sample. METHOD: Method: EG&G, Bionomics protocol entitied "Protocol for Flow-through Toxicity Tests with Fishes," January 2, 1980. Test type: Flow-through acute GLP: No Year Completed: 1981 Species: Fundulus heteroclitus Supplier: Commercial supplier Analytical monitoring: Temperature, pH, DO, and salinity Exposure period: 96-hours `Statistical methods: LCs values could not be calculated. Test fish age: Juvenile. Length and weight: Loading: 0.092 g/L. Length = 27 -- 35 mm with a mean of 31 mm Weigh=t 0.28 --0.g6wi3th a meanof 0.4g6 Pretreatment: Not noted. Test conditions: Dilution water: Natural, filtered seawaterfrom Big Lagoon, a Gulf of Mexico estuary, FL. or Dilution water chemistry: Salinity: 27 28 parts per thousand 001672 Lighting: Fluorescent lights provideda daily photoperiod of 12 hours light and 12 hours dark with an intensity of 1,100 lux incident to the water Ssutrofcacke.and test solution preparation: A primary stock solution of V5o0l2u,m0e0t0rimcgf/lLaswkaasndprberpiangriendgbtyo vadodliunmge5w0it2hgdreaimosniozfetdewsattsear.mpAlle ttoesat 1-L solutions were prepared by adiluterdelivering five nominal concentrations of the test sample and control water. Flow-through rate: Approximately 1.5 aquarium volume replacements Sptearb2il4ithyoourfst.he test chemical solution: Not noted. Exposure vessels: 30 x 30 x 91 cm glass tanks containing ~50 Loftest solution volume. Number of replicates: two NNuummbbeerr ooff cfiosnhcepnetrraretpiloincsa:te5: p1l0us a blank contr-ol Water PchHermiasntgrey(d0u-9r6inhgoutrhse):study: 77..48.78..90 ((c2o0n0t0romlge/xLpoesxuproes)ure) Temperature range (0-96 hours): 22 27C (for all aquaria) Dissolved oxygen range (0-96 hours): 05..67- 6-- .6.89 mmgg//LL ((c2o0n0t0romlge/xLpoesxuproes)ure) Salinity range 27 -- 28 p(a0r-t9s6pheorutrhso):usand (for all aquaria) Remarks: During the third day of exposure, the diluter stopped cycling and resulted in only 6 cycles (1 L solution /cycle)forthe 24 hour period. Since the test concentration did not change, it was concluded that this did not affect the validityof the test. RESULTS Nominal concentrations: Bk control, 125, 250, 500, 1000, and 2000 mg/L Elementvalue: 24-hourLCs: 48-hour LCs: 72-hour LCs: 96-hour LCs: >2,000 mg/L. >2,000mglL 2,000 mg/L >2,000mglL Element values based on nominal concentrations. sRuebmsatraknsc:e Treesmtairnkgswfaiesld.coTnhduecvtaeldueonretphoertmeidxtauprpeliaessdteostchraitbemidxitnurteheatnedst not the fluorochemical proportion alone. 001673 CONCLUSIONS The FC-206C 96-hour LCso for Fundulus heterociitus was determined to be >2,000 mg, the highest concentration tested. 10% mortality was. observed at this concentration. Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 DATA QUALITY Reliability: Kiimisch ranking 2. The study meets all criteria for quality testing. However, sample purity was not properly characterized and the study lacks analytical confirmationofthe amoo ffluu orocnhemitcal proportion in the solution. Additionally, D.O. concentrations fell significantly below acceptable levels. REFERENCES This study was conducted by EG&G, Bionomics of Pensacola, FL at the requestofthe 3M Company, 3M Lab Request number 7038, 1981. OTHER Last changed: 6/26/00 001674 EAL# Sl21% LR# 703% Acute toxicity of a surfactant solution to the mummichog f(Fluonud-utlhursouhghetseyrsotcelimtus) in a Sl-2/% Fc-206 C 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. oo M1a0r3i07neGRulefseaBrecachhLHaibgorhawtaoyry Pensacola, Florida 32507 September 1981 u3 Hof 001675 MarineEGR&eGseBaricohnomLiacbsoratory P1e0n3s0a7coGlual,f BFleoarcihdaHigh3w2a5y07 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: TBoMxRiL'cSitTyesTtestPsrotwoictohl:Fish"ePsr"otocol for Flow-Through Test animal: Mummichog, Fundulus heteroclitus Source and age: Commercial supplier, juveniles Seawater: Natural, filtered, 27-28 parts per thousand salinity Solvent/carrier: None ~ ENfomfiencatl:crtietsetricoonn:cenMtorarttiaolnist:y. 1(m2g5),/215i0te,r50(02,) 1,000, and 2,000 i milli2 grams 96-hour LC50: C2o,u0l00d mngo/ttbe calculated; maximum mortality was 10% in : 001676 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 LCS0 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 recei: on 12 August 1981 in one 9.5-liter (&) cubetainer labeled|"3M SAMPLE 81-2/8."| The test material, 2 deep orange-yellow liquid, waf s or 55 re eceiv] ed: All test concentrations are reported here as milligrams (mg) of surfactant solution per % of seawater. or as parts per million (ppm) . . Test animals Mumnichogs were purchased from a commercial supplier and maintaine 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 degree: Celsius (C). period. No mortality was observed during the entire holding : The control fish were 27-35millimeters.(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. 0016777 2 Test water Water used to maintain and test the fish was natural seawater whic 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 l0-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 @iluter cycled only 6 times in 24 hours because of a malfunction. The cycling rate of 3.2 ycles/hourprovided-approximatel 1.5 volume additions in 24 hours. v The surfactant stock solution (502,000 mg/%) was prepared by weighing 502 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-% glass reservoir attached to a "dipping bird" (Mount and Brungs, 1967). A 15.5 milliliter volum 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 0016784 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 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. piluter 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 ` 001679 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 108 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 <508. Physical or behavioral abnormalitieswere observed onlyinthe 2,000 ppm test concentration. After 24 hours of exposure, 4 fish were observed to be darkerthannormal, however, this was observed again only after 96 hours when 1fishwasappadarrkeertnhat nnolrmy al. `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 oxygenconcentrations. 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 and72 hours ofexposure, especially in the 2,000 ppm test concentratior The low DO may have been caused by a high oxygen demand after 48 hours and thelacckh ofangeduoriv ngdeayr3. The pH was 7.4-8.0 in all test containers throughout the exposure (Appendix A). = 001650. 5 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. : z 001681 6 TABLE 1. Macoornstcuaerlnfitatcrytaatoniftonmssuomlamruietcihogonigvseinn (afFsluonwndiounmlguisnanlahteutceroranolccelnsitetaruwasat)tieorne.sxpoofTseesdtto whole material. ConcenNotmriantailon Control 125 250 500 1,000 2,000 (mg/t;pp)m) - Thom TeMeortalityTh h(sel 35 ow 0 0 To 0 0 0 0 o o 0 "0 0 0 o 0 o 0 0 0 0 ! 001682 PREPARED BY: 7 G. Scott Ward SS&tSudySDeirtehctorWon 28 Shatie n AUDITED BY: Alan G. Miller Qu(ali,ty NAsseurance UAIE 28 Dat1e 9 Rav ata await: _ 19 Sulky 1581 Preliminary report audit:18d. Final report audit: <4 7% REVIEWED AND APPROVED BY: Peter J. Shuba, Ph.D. : DTecShnical Q ChoraS inator 25Datd e 001683 E65 BioNomics Sng rs _-- APPENDIX A A-1 mCoH.oE:eCTIpVEe:ToDRercomter 1980 CLIENT: 3M Company PROJECT NO:R36 a sions worn $-2o-81--S4 semecro 3 oilra C_ OLESTIOVAECEIPTs106aFeoR &34 hTA SPECIES: Fundulus heteroclitus : TEST MATERIAL: Surfactant solution i DATE MAINTENANCE/ACCL IMATION Bcan:_20 AUG covorTion os vam: Excellest YLOIFRETASLTIAGTEY:(44) TA sce roe 10.34. 40oHrO_S,VJouPvRbIEemOanRbineTloeTL,EoSTcING-- ron awk own Dram [8 TEw oRmen s est srsron PE [RerimiveJ|rocm 771530|m@-| Doo Kase weaor psycomanen | Ewweisan6esvieisto | Test owas vouse (1) | owen vows (1) | sawiny oon) i " po@a- [w@e- [rveenGI[enn GD| meer FrasToto: BritTsh Prolue. of eo hea - Aviad Ae Cat ore: TEST TERIAL 75 ACTIVE INREDIENTANAE MATERIAL Sov cin sTnor ceonsan, Jefseoy TOLL [TT DRrSaEnk woot or crenicassroc roo(| wn[wa] IT Tre cocenarion sto soariov uso 0, 2-3) wafon]| LTTTTR HOUR GF SOLVENT ABE on) [on[onf[ ur]w nnfa usefrJe oa unr] TODITION COATS: (DOGO nt DEVIATIONS AEM PROTO) - Ga. 001684 | Asses sovouics r ew Lelee rELar ryLy| eI he B [5o % owr ] ea Lan[oSx]r LLf%eLL u LLaL s> T |n T e2e | wm EE [[ellieet]ustbboodd o67J6o[17C9 udntd657/50[[773l7zd5m9el8--67706[57t85e3no5n7s0eT1I7E5 [oaes [h T Tlialus Bdo/T 6mine c/ ase e o/oTpittheT [a67e 0a 15dT sderoosoeTht CF2ele[lalaimlbiaTbeelrleoe/roemEaPlrtsoSfsGohTi TTTSeo/foeFl eabe roeefeeiy eT Tok : tases pe5 ero pa2 of re[2913s B[R BRa ETToo) T 13dyr a a THAE e DCo ECR ffrroomme y CHa a200r 0 y 400 4 Lgl [MREETR ||s evS i e ewn iarp e a Sere rFoag] a-- SE ERE me oe > BGiEl El melen FmEe R CLARHen BEST COPY AVAILABLE | I3