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AR 226 - 0723 ACUTE TOXICITY TO AQUATIC INVERTEBRATES (GRASS SHRIMP) IESTSUBSTANCE ~~~ 0000000 Identity: A mixture containing perfluorooctanesulfonate, which may also be referred to as PFOS, FC-95,or as a component of FC-203. "Octanesulfonic acid) (CAS # 2795-39-3). Remarks: The 3M production lot number was 1. The test sample is FC- 203. Current information indicates it is a mixture of 1.34% PFOS, 35% diethylene glycol butyl ether, 37.85% water, 20% ethylene glycol, 2.66 % !" Sultone foamer, 3% sodium octyl sulfate, 0.1% sodium lauryl sulfate, and 1 0.05% tolyltriazole. The following summary applies to a mixture with incompletely characterized concentrations of impurities. Data may not accurately reflect toxicity of the fluorochemical component of the test sample. M0 ETHO0 D: 00000000 Method: Methods for Acute Toxicity Tests with Fish, Macroinvertebrates, and Amphibians (U.S. EPA 1975). Type: Acute static GLP: No Year completed: 1979 Species: Palaemonetes pugio Supplier: Field collected from Big Lagoon, a Gulf of Mexico estuary adjacent to the laboratory, Pensacola, FL. Analytical monitoring: Temperature, pH, salinity, and DO Exposure period: 96-hours Test organism age: 16-22 mm rostrum-telson length Statistical method: ECs values calculated using the Stephan computer program, 1977 and 1978. Test conditions: Dilution water: Filtered natural seawater, from Big Lagoon, FL - Dilution water chemistry: Salinity: 25-26 ppt Temperature: 22-25 C Lighting: Not given. Stock and test solution preparation: Exposure concentrations prepared by direct addition of test substance. Exposure vessels: 19 L glass jars containing 15 Lof test solution. Number of replicates: 2 Number of organisms per replicate: 5 Number of concentrations: five plus a blank control Water chemistry during the study: Salinity range: (0-96 hours): 26 ppt Temperature range (0-96 hours): 22 C 000588 pH range (0-96 hours): 7.88.0 (control exposure) 7.58.1 (1000 mg/L exposure)" Dissolved oxygen range (0-96 hours): 4.86.4 mg/L (control exposure) 12-63 mglL (1000 mg/L exposure)" *be1c0a0u0semgth/eL h(isgehceosntdcohnicgehnetsrtactoinocnernetsrualttieodn)inetxoptoalsumroretvalailtuyebsyu7s2ed hours. RESULTS 000 Nominal concentrations: Bk control, 220, 360, 600, 1000, and 1800 mg. Element values: 96-hour ECs = 510 (360 - 740) mg/L Element values based on nominal concentrations Remarks: Testing was conducted on the mixture as described in the Test Substance Remarks field. The values reported apply to that mixture and not the fluorochemical proportion alone. conclusions The test substance 96-hour ECs, was determined to be 510 mg/L with a 85% confidence Interval of 360 to 710 mglL. Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 p0 atAQuau0 TY 0000 Reliability: Kiimisch ranking = 2. This study meets the criteria for quality testing. However, sample purity was not properly characterized and the study lacks analytical confirmation of the amountoffluorochemical proportion in the ~ solution. REFERENCES 0000000 Test was conducted by EG&G, Bionomics Marine Research Laboratory of Pensacola, FL at the request 4971S, Sample 7902, 1979. of the 3M Company, Lab Request number o0 mer 000 Last changed: 6/27/00 000589 3) Ascaumtpele t7o9x0i2cittyo gofras3sM Csohmrpiampny's (Palaemonetes pugio) Fe-203 LA) LR 497) S EAT 79295 Toxicity Test Report Submitted to ) 3M Company St. Paul, Minnesota Project Number H90-500 Report Number BP-79-8-121 / EG&G, Bionomics Marine Research Laboratory Route 6, Box 1002 PAeungsuasctol1a9,79 Florida 32507 000550 | 1 A marine toxicity test was conducted at Bionomics Marine : Research Laboratory (BMRL), Pensacola, Florida, to determine the acute effect of 3M Company's sample 7902 on grass shrimp (Palaemonetes pugio). The criterion for effect was death. Results of the test are expressed as 24-, 48-, 72-, and Geohour1c50's. (the concentrations of the test material estimated to be lethal to 50% of the test animals at the specified times). All data related to this test are stored at BMRL. + MATERIALS AND METHODS | Test material The sample was received at BMRL on 3 July 1979, and was contained in a 500-milliliter (mf) NALGENE bottle labeled "3M SAMPLE 7902, BIOASSAYS: 96hr LCS50-GRASS SHRIMP (PALAEMONETES VULGARIS); 48hr ) LCSO-ATLANTIC OYSTER LARVAE (CRASSOSTREA VIRGINICA)." The sample was a medium orange liquid. Concentrations are reported here as milligrams (mg)of`whole test material per % of seawater or as parts per million (ppm). Test animals Grass shrimp, 16-22 millimeters rostrum-telson length, were collected from Big Lagoon, a Gulf of Mexico estuary adjacent to BML. The shrimp were held in the laboratory in flowing, natural seawater. During the 48-hour period prior to testing, salinity was 25-26 parts per thousand (/oo) and temperature, 22-25 degrees Celsius (C). No mortality was observed during the holding period. It should be noted that Palaemonetes pugio were tested instead of J PB. vulgaris based on approval of Dr. Eric Reiner, 3M Company. 000591 2 Test water ) Water used for holding and testing was natural seawater which was pumped from Big Lagoon. The pump intake was 85 meters (m) off- shore at a depth of approximately 3 m. Test water was pumped by a #316 stainless steel pump through hard polyvinylchloride (PVC) pipes, through sandfilled fiberglass filters, and through l0-micrometers (um) pore size polypropylene core filters into an elevated fiberglass reservoir. Water was continously and vigorously aerated in the reservoir and flowed by gravity through PVC pipes into the laboratory. There it was pumped through a 5-um pore size polypropylene core filter and distributed into test chambers. The chemical composition of BMRL seawater is characterized in ) Pependix A. Test conditions Methods for the 96-hour static test were those described in . Methods for Acute Toxicity Tests with Fish, Macroinvertebrates, and ; Amphibians (U.S. EPA, 1975). The test was conducted in 19-1 uncovered glass jars which contained 15 of filtered natural seawater. Salinity was 26 /oo and temperature was maintained at 22C. Five _ shrimp were tested per jar and all treatments were duplicated. There was no aeration. Dissolved oxygen (DO) concentrations were near 90% of saturation at initiation of the test. Based on a range-finding test, shrimp were definitively tested at nominal concentrations of 220-1,800 ppm. Test concentrations were prepared by adding appropriate weighed amounts of sample 7902 directly ) into seawater in the test containers. No solvent/carrier was used. The seawater control received no test material. 000592 3 3 Test animals were not fed during the definitive test which ) was conducted 8-12 August 1979. Statistical analyses Based on the results of the test, 48-, 72-, and 96-hour LC50's and their 95% confidence limits were calculated. The computer program (Stephan, 1977 and 1978 personal communication) estimated LC50 values by using one of three statistical methods in the following order: 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. The computer scanned the data, identified the most suited method, and | performed the analyses. For this test, the moving average angle method , was used to analyze the 72- and 96-hour data and the probit analysis method was used for the 48-hour data. RESULTS AND DISCUSSION . 3M Company's sample 7902 was "practically nontoxic" to grass ' shrimp, based on EPA Hazardous Substances Guidelines, FEDERAL REGISTER, 30 Dec 197e 5. n Theb calceular ted 96-hour LCSO was[510 wppi m t95h 8 confidence limits of sosn ne 1) After 96 hours of exposure, nortalityrangedfrom 03 Tn The COREFST ES 100% in 1,800 ppm (Table 2). LowDOconcentrationscouldhavecontributed to thetoxicityof sample 7902. At 24 hours of testing and later, the DO concentrations generally decreased as the test concentrations increased and after 96 hours ranged from 16% of saturation in the 1,000 ppm test concen- , tration to 66% of saturation in the control (Table 3). Loading of 000593 +0 4 test animals (0.013 g/2) was not sufficient to cause the low DO ) concentrations as evidenced by the 66% of saturation measurement in the control after 96 hours of testing. Apparently two factors, the inherent chemical nature of the test material and the increased oxygen demand of shrimp stressed by exposure to sample 7902, resulted in the low DO concentrations. The pH in all treatments was within an acceptable range. After 96 hours, pH was from 7.5-7.8 (Table 3). . ) J 000594 : 5 3 REFERENCES Stephan, C.E. 1977. Methods for calculating an LCS0. ASTM, Aquatic Toxicology and Hazard Evaluation, ASTM STP 634. F.L. Mayer and J.L. Hamelink, eds. pp. 65-84. U.S. Environmental Protection Agency. 1975. Methods for acute toxicity tests with fish, macroinvertebrates, and amphibians. EPA-600/3-75-009. 61 p. ) 0005395 sf 6 3 TABLE 1. Cexaplocsueldatetdo I3CM50C'osmpafnoyr'sgrassasmplsehri79m0p2I(sPnatlaaetmoinecte,sunpauegriaot)ed Vsaelauweasterw.ereScaallicnuitlyatewadsba26sed/ooon naonmdintaelmpecroantcuernet,rat2i2oCn.s of whole material. Hour 150 (mg/2;ppm) 2a >1,800 48 2,400 72 570 96 510 95% confidence limits (ng/%) -- --- 410-790 : 360-710 ) TABLE 2. Mtoort3a4liCtomypaonfy'gsrasssampslherim7 p (9 iPanlSa0 etmaotni2 ect,esupnuageiroa)tedexpsoesa-ed wTaetsetr.concSeanltirnaittyionwsasar2e6 gi/ovoenanads wtheomlpeermatautreer,ial2.2C. conNcoemnitnraaltion Mortality (3) : (mg/%;ppm) mE fh JR TEE control 0 0 0 220 o 10 10 10 360 0 0 40 0 600 0 o 30 0 1,000 0 20 80 50 1,800 0 50 100 100 J) 000596 Le 7 y TABLE 3. Mueraisnugreda 9c6o-nhcoeunrtraetxipoonssureofofdisgsroaslsvedshroixmypgen(PaanldaepmHonetes pduugcitoe)d itno s3tMatCiocm,paunny'aserastaemdplesea7w90a2t.er.TheSaltiensittwyaswascong2i6ve9n/00asawnhdolteemmpaetreartiuarle., 2D2iCs.solvTeedstoxcyognecnenctornacteinotnrsatairoens Tahree ptHhewaasvemreaagseuroefdmeiansuRreepmleinctasteiAn oRnelpyl.icates A and B. conNcoemnitnraatlion og/tipg Control 20 | 360 600 1,000 , Lew TOR 6.4 (83) 6.2 (85) 6.3 (86) 6.4 (88) 6.3 (86) 6.4 (88) mg/Diis(s8oolfvesdaotxuryagteinon) 24K 8h _72h 6.0 (82) 6.0 (82) 5.8 (79). 5.6 (7 5.0 (68) 3.8 (52) 5.2 (71) 3.8 (52) 2.2 (30) 5.4 (73) 3.6 (50) 2.2 (30) 5.0 (68) 2.4 (33) 1.4 9) 4.8 (66) 1.8 (25) 1.0 a4) 96h 4.8 (66) 2.8 (3) 1.6 (22) 1.6 (22) 1.2 16) 2 No measurement because 100% mortality had occurred. pH Oh 9%h 8.0 7.8 8.1 7.7 8.0 7.6 8.1 7.6 8.1 7.5 81 2 J 000597 APPENDIX A D RCeshualrtasctoefriCzhaetmiiocnalofAnSaellyescetsedfCorhemRiocuatline ConstituentsLaibnorBaitoonroymicSseaMwaartienre Research Constituent. JanCounacreyntratio157n9 .14 June7 I ACrasdenniiucn <00..000012 <00.l00016 CChorpopmeirum 00..0020375 0<0-l0011 MNeircckuerly 00..002007 <<00..001005 LZeiandc 00..00051 - <<00..0022 ATmomtoanliaPhNoistphraotgeenaassPN <00..0422 <00..0124 NNiittrraittee NNiittrrooggeenn aass NN <00l.0011 <00--0011 TSoutlaflidePsetroleun Hydrocarbons. a<l5.o0 <l5.o08 PPeosltyicchildoersinated Biphenyls NNoonnee ddeetteecctteedd? NNoonnee ddeetteecctteedd eeeeres ene eet WLaatbeorratsoarmyplesseawwearteercoslylsetcetmedaftferromtBheiomnioxmiincgs `MsatraitnieonReisneatrhech wet lab. pesticides: BaHlCd,rinl,idnidealnder,inh,epteancdhrlionr,, pheretphtaanceh,lorDDEe,poxTiDdEe, (DDD), DDT, methoxychlor, endosulfan, Strobane, v; : toxaphene, `kelthane, and chlordane ail <0.005 vg/%. . Peolychlorinated Biphenyls: A1r2o60c,lor1e2211,0161,2421,232a,nd1214285,4 - . 211 0.05 yg/t. CPetroleun hydrocarbon sample collected 10 July 1979. 000598 Lo Loe 3 PREPARED BY: AUDITED BY: ) REVIEWED BY: APPROVED BY: ) o Tom Heitmuller Study Director G3 Scott Ward QGua.litSy AssuranWce aUnsit Peter Shuba, Ph.D. * --Jes Shes Project Coordinator Rod Parrish biector nel. ~ 000599