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ACUTE TOXICITY TO FISH TEST SUBSTANCE Identity:A mixturecontainingperfluorooctanesulfonatweh,ich may alsobe referredtoas PFOS, FC-95, or as a component of FC-185F. (1Octanesulfonicacid)(CAS # 2795-39-3) Remarks: The 3M productionlotnumber was 1-2303. The testsample is FC-185F, cc 817-19. Currentinformationindicatesitisa mixtureof4% PFOS, 36% diethyleneglycolbutylether,29.29% water,14% ethyleneglycol, 8% Sultonefoamer,8.35% sodium octylsulfate0,.3% sodium laurylsulfate, and 0.06% tolyltriazole. The following summary applies to a mixture with incompletely characterized concentrations of impurities.Data may not accurately reflectthe toxicityof the fluorochemkal component of the testsample. METHOD: Method: ASTM-E729-80 Type: Staticacute GLP: No Year completed: 1982 Species: Pimephalespromelas Supplier:Dale FaftigFishFarm, Brady,NB Analyticalmonitoring: Temperature,pH, and DO Exposure period: 96-hours Statisticamlethods: LC50 valuescalculateudsingboth moving average angle and probitprograms inconjunctionwiththe 3M TRAC Computer system Test fishage: Juvenile Length and weight: Average length 38 mm Average weight 0.38g (wet) Loading: 0.48g fish/L Pretreatment:None Test conditions: Dilutionwater: Carbon-filterweedllwater Dilutionwater chemistry: Hardness: 252 mg/L as CaC03 Alkalinity: 225 mg/L as CaC03 Lighting:A dailyphotopedod of16 hourslighatnd 8 hoursdarkwitha 30 minute transitiopneriodwas maintainedthroughoutthe testingpedod. Stock and testsolutionpreparation: Test solutionswere createdby direct individuawleight additions. Concentrations dosing rate: Once StabiliotfythetestchemicalsolutionsN:otnoted Exposure vessels: All-glasasquaria,35x2Ox25 cm containin1g6 literosf testsolution Number of replicates: 2 Number of fish per replicate:20 Number of concentrations: fiveplus a blank control Water chemistry during the study: pH range (0-96 hours): 8.0 - 8.2 (controlexposure) 7.7- 8.2 (370 mg/L exposure)* Temperature range (0-96hours): 17 -21 OC Dissolved oxygen range (0-96hours): 5.8- 9.2 mg/L (controlexposure) 1.3- 9.3mg/L (370 mgll exposure)* 370 mg/L (second highestconcentration)exposure values used because the highestconcentrationused resultedintotalmortalityby 24 hours. Remarks: The dissolved oxygen concentrationwas below 60% saturationin allexposure concentrationsexcept the controlby 48 hours. This may have contributedto the observed mortality. RESULTS Nominal concentrations: Bk control,100, 155, 240, 370, and 560 mg/L Element values: 96-hour LC50 = 344 (318 - 376) mg/L Element values based on nominal concentrations Remarks: Testing was conducted on a mixtureof as described in the Test Substance Remarks field.The values reportedapply to thatmixture and not the fluorochemicalcomponents alone. CONCLUSIONS The testsample 96-hour LC50 forfathead minnow was determined to be 344 mg/L with a 95% confidence intervalof 318 to 376 mg/L. Submifter: 3M Company, Environmental Laboratory,P.O. Box 33331, St. Paul,Minnesota, 55133 DATA QUALITY ReliabilityK:Jimischranking= 2. Testing meets the criterifaorqualitytesting. However, sample puritywas not properlycharacterizedand the study lacks analyticalconfirmationof the amount offluorochemicalproportioninthe solution. REFERENCES Test was conducted by the 3M Company, EnvironmentalLaboratory,Lab Request number 7544,1982. OTHER Last changed: 6/26/00 I orm -11-C TECHNICAL REPORT SUMMARY D &to 2/l/82 .tO: TECHNICAL COMMUNICATIONS CENTER - 201-2cN (Important- Ifreportisprintedon both sidesof paper,send two copiesto TCC) See "GuidelinesforCompletion of TechnicalReport Summary" availablferom InformationLiaisonor TCC (3-5545). Division Dept Number Environmental Project Laboratory (EE & PC) 0535 Prol*ct Number Colpmercial Report Title Chemicals 9972210100 Report Number Aquatic Toxicity Testing: FC-185F (cc8l7-19) L 1-2303 LR 7544 007 To E. A. Aghro_ Reiner A. N.*&Iter - Notabo4ok Reference 2-3E Employee Numberis) 09362 No. of P"es Including Coversh"t SECURITY 10. 13 ooon 0 cloud KEYWORDS: IncludLeabCode 4OR R E(JeefefSJMRCEJITV E ne the acute varying concentrations 3M CHEMICAL REGISTRY Now ChwnicalRseported 0 Yes Ki No aquatic LC50, followin ex3osure to of FC-185F (CC817-19) Lt -2303. EE & PC-Div. (Env. Lab) Toxicity (Aquatic) REPORT ABSTRACT: Company R&D. This abstractinfomwtion isdistributebdy the TechnicalCommunications Center to alert3M'ers to The acute static aquatic 96-hour LC50 values obtained for r,-ithc.acmlinnows (PimLph,-il(--sprom(--las) followinq L-xposure to FC-185F in replicii-te-d experiments were 339 (not defined) and 372 (333-415) mg/l. The combined.96-hour LC50 was 354 (0) (not defined) mg/l as calculated using the probit analysis statistic. @Data generated limits include LC50 values with 95% confidence Information lnitialc FC-185F/ANW Page 2 February 1, 1982 CONCLUSIONS In these replicated 96-hour LC50 aquatic tests, the calculated values for fathead minnows (Pimephales promelas) were 339 and 372 mg/l. Materials possessing an LC50 this order of maqnitude are considered to be practically nontoxic based on the NIOSH criteria for aquatic toxicity interpretation. (2) II]TRODUCTION The test substance is a foamy, clear, dark amber liquid, soluble in water at ambient room temperature. Tests performed on this material evaluated its potential aquatic toxicity and the data generated form the basis of this report. ACCLTMATION AND EXPERIMENTAL DESIGtl The test protocol utilized for this study was modeled after that described by ASTM-E729-80. (1) The fathead minnows (Pimephales promelas) were obtained from a private hatchery (a). Stock E71-sh-wereheld in a flow through system fiberglass holding tank filled with carbon-filtered well-water at 14-16 degrees C. A daily photoperiod of 16 hours light and 8 hours dark, with a 30-minute transition period was maintained throuqhout the acclimation and testing period. The fish were fed Tetra-Min (b) daily, food being withheld 48 hours prior to and throughout the test period. Fish were acclimated to test temperature for 2 days prior to use in assays. Twenty (20) fathead minnows, uniform in size, were tested at each concentration of chemical. All-qlass aquaria, 35x2Ox25 cm containing 16 liters of diluent plus toxicant comprised a study chamber. Test fish were randomly allocated to each test chamber within 30 minutes followinq toxicant addition. The fathead minnow experiments were conducted at 19+2 degrees C. Mortality, temperature, dissolved oxygen level, and pH of- all test solutions were measured at 24-hour intervals or until total mortality had occurred. General observations were recorded relative to swimminq pattern and behavioral chanqes induced by exposure to the test chemical. The acute short-term static bioassays were performed on FC-185F using carbon-filtered well water of known composition and constant quality as the diluent (Tables li2). a) Dale Fattig Fish Farm, Brady, Nebraska. b) Commercial Fish Food of known composition. FC-185F/ANW Page 3 February 1, 1982 The 96-hour fish studies were performed in replicate usinq the following FC-185F logarithmic concentrations: 100, 155, 240, 370, and 560 mq/1. This range of dilutions was selected to bracket 96-hr LC50 values predicted from preliminary exploratory toxicity tests. LC50 values with 95% confidence moving average angle and probit TRAC Computer system. limits were calculated usinq both programs in conjunction with the 3M Monitorinq equipment used included ASTM thermometers, temperaturr=--compensating pH meter, a Yellow Sprinqs meter, and a Taylor temperature chart recorder. Orion dissolved oxygen RESULTS The fathead minnows (Pimephales promelas) used in these studies had an average weight of 0.4 grams and a---fe--ng-otf-f3f.8 cm. The loadinq factor was 0.48 g/l; the maximum recommended loading factor is 0.8 g/l (1). Temperature, pH, and dissolved oxygen values and ranges obtained during this study were: 19+ 20C, 7.7-8.2 pH units, and 96-hour dissolved oxygen values raniied from 1.3-5.9 mq/1. These latter values calculated out to a minimal oxyqen saturation of 14-63%. In this replicated study, the fish 96-hour LC50 values were 339 and 372 mq/1. Chemical possessinq an LC50 value in this ranqe are considered to be slightly toxic to the aquatic environment (2). The data reported herein are based on studies performed by 11. T. Elnabarawy and R. R. Robideau. Accompanying data sheets comprise original data. A copy of this report is filed in the Environmental Laboratory Archive System, Building 2-3E. It should hf- noted that the qenerated results were reported in the absence of information relative to the "purity" and the "stability" of the chemical substance. The reporter] LC50 values were calculated on the basis of the "observed mortality rates" and of the calculated initial concentrations of FC-185F in test solutions. REFERENCES (1) ASTfi-Standard Practice E729-80. Standard Practice for Conductinq Acute Toxicity Tests with Fishes, Macroinvertebrates, and Amphibians. American Society for Testing and Materials, Philadelphia, PA 1980. (2) Registry of Toxic Effects of Chemical Substances, 176 Edition, Christensen, H. E., and E. J. Fairchild, Eds., p. XV and Ci, U.S. Department of Health, Education and Wt-.1fare;National Institute for occupational Safety and Health, Washington, D.C. (June, 1976). TABLE 1 WELL WATER QUALITY SAMPLE DATE: 1/28/82 SAMPLE TAKEN: 3M Bldg. 2-3E, St. Paul SAMPLE DATE 1/28/82 (TAKEN FROM ROOM 5) PARAMETER CONCENTRATIO17 ENV. LAS WATER QUALITY BOOK REF. pll Residual Chlorine Ammonia Nitrogen Conductivity M-Alkalinity Total Solids Total Hardness Total Fluoride Dilute COD Total Coliform Standard Plate Count 7.7 8 <0.02 mg/l 9 <0.1 mg/l as N 8 330 umhos/cm at 250C 9 223 mg/l as CaC03 8 315 mg/l 8 252 mg/l as CaC03 8 <0.02 mg/l 9 <0.4 mg/l 9 Negative 10 21 per ml 10 Aluminum as Al* 0.2 mg/l 14 Arsenic as As* <0.005 mg/l 14 Boron as B* <0.2 mg/l 14 Cobalt as Co* <0.02 mg/l 14 Copper as Cu* <0.02 mg/l 14 Chromium as Cr* <0.03 mg/l 14 Cadmium as Cd* <0.01 mg/l 14 Iron as Fe* <0.02 mg/l 14 Nickel as Ni* <0.02 mg/l 14 Lead as Pb* <0.05 mg/l 14 Silver as Ag* <0.02 mg/l 14 Zinc as Zn* 0.05 mg/l 14 Mercury as fig* <0.2 ug/l 14 PCBIS** ND 95 Total Organochlorine** ND 95 Pesticides Total ND 95 organophosphorus** Pesticides Sample Date 1/28/81 **S ample Date 3/4/81 TABLE 2 ENVIRONMENTAL BLDG. ST. PAUL, LABORATORY 2-3E MINNESOTA FOURTH QUARTERLY REPORT, 1981 WELL WATER SUPPLY FOR AQUATIC MLOXICITY TESTING PARAMETER TOTAL HARDNESS* as mg/l CaC03 TOTAL "M" ALKALINITY* as mg/l CaC03 ELECTRICAL SPECIFIC CONDIJCTANCE* as umhos per cm2 at 250C TOTAL SOLIDS* as ing/l pii** NOV 2 248 228 330 320 7.6 NOV 30 252 DEC 29 256 AVERAGE (+ S) 252 + 4 226 221 225 + 4 340 380 350 + 27 300 308 309 + 10 7.6 7.7 7.6 + 0.1 STANDARD PLATE COUNT*** per 1.0 ml 2 10 27 13 + 13 CRITERIA OF CONSTANT QUALITY Monthly ranges should be less than 10% of their respective averages. (ASTM Standard E729-1980.) Monthly range of pil should be less than 0.4 unit. E729-1980.) (ASTM Standard Total bacterial densities should not be greater than 500 organisms per ml. (USEPA-600/8-78-017, p. 101.) ENVIRONMENTAL LABORATORY AQUATIC TOXICITY DATA SHEET DEFINITIVE (FULL-SCALE TEST) LR De Tes--!RlQgVK. &UTF SftrMaterial Test edF r-j&sE-w-Bil--L9-1-ot -st Organi-m-Fitnr=At-mi-mrcme-:&@.5oRAaMsou_MER.Date Recld 11/no JAL_Satch 1I g.Wt.0, 5&granis Avg. Size_5LB_= No. Orgarusms per dose_,Zo Loading FactorA L4$; g/l .sh Disease TreatTient:_Ll-!DMC- @st SolutionVolume 1(6_Liters/All-GlassTank Tank Dimensions: 35x2O an and 25 an deep -me Started :P" Date Started Z_j Date Canpleted -lutionWater Carbon-filteredwell water (Tenp. -C., D.0. ppn, pH ivestigator.z@:@@C-@ LC 50 (9(5M%oCoUnKfidence Lim-its) @ullSignature)PROIB@trAN*&.YsLs 1-"9 cy)s 0-,omi D:N) MOVItJi@ AVERAfiE ,ank InitialTotal ANfiM Mtl"m 24 Hours SWIL4 (2-Ctto48 Hours wxg 7 @0. Conc. Amount Total No. pH D.O. Total No. pH ID.O. Total No. pH D.O. Total No. pH D.O. mg/i Added Dead PPM Dead ppm Dead ppm Dead pprn Cont:rui 0 Ili I ckL n 0 0 0 -"u'q 10 -0 0 C) 0 1.4 2, 9 2-,1 ZLL /a 0 0 A/ 20 2-() Test TenTp.OC Initi.al&s Date m@Tne@n :4k-liiftut AALI %Ll4/-2ZZ!2 Liqll%r), ALIIF%LC- ILI 1,1 2condaryEffects (otherthan Mortality): rank No. Symptans or Reactictis Dntrol: 24-Hr. 4tT -w-3;0"K EC50 Total Number Affected 48-Hr. 72-Hr. 2^ f3- as 63VAM fl ki9-- LIIE 4 flu 2_1qo arm5azA 96-Hr. c-- ENVIRONMENTAL LABORATORY AQUATIC TOXICITY DATA SHEET DEFINITIVE (FULL-SCALE TEST) LR pe Te-stginiAm, Material Tested_EC-W?@ S_Fm Atti-icIT-ot I- 4,W)m @st organism_r_p_ggg&D__@@@Source @ WES@:A Date Rec Id rg.Wt. -0@grairs Avg. Size % j,.g an l@b.organisms per dose_2_CLLoading Batch P2,) 84,46-1m) Factor g/l i-shDisease Treatment: hlomjfast Solution VolLune_VD_Liters/All-Glass Tark Tank Dimensions: 35x2O an and 25 an deep -me Start ed_Jll_t@I)ate Started. 1.]ZIDIS2-., 1-lutionWater Carbon-filtered well water (Temp. - - Date Ccrnpleted_4L VA& C. I D.0... pprn pH_I?.Z.) ivestiga ---KA LC (995%Z= -ull Signature) -;R6iaA%NTALYSIS mo\jl ri A\VTE ANC-T@ mErAm SWC73.@-MOw-4-t Lank Initial Total 24 Hours 48 Hours \@0. Conc. Amount Total No. D.O.lTotal No. pH mg/i Added Dead ppin Dead 1 ence Lin-Ltis) CoR&uen 72 Hours -D.O.lTotal No. pH ppm Dead i@ (kioUt-im Lp@D0*4 96 Hours D4.:mO. Total No. pH D.O. ppm Dead pprn w@i ax Control 0 5,9 11)0 -VaQf) I-s;:z 0 :-2zb LM CC)) riI c:> -,c@ di,q P3 4/.-11@ Test Temp. OC 1.7 Initials & Date cmTients:.L*=UmljlrAJkALI 'O)t@L4jALC-- im AMRICtxr -condary Effects (other than Mortality): -rank No. Symptans or Reactions o,no4notro1l' 7 24-Hr. @Jr+i Nw e- 0 5 1/-2R 20 oe-" ZaL-3. //@22 DAZE - EC50 Total Number Affected 48-Hr. 72-Hr. -AJLIAtg AloAj r,@ 157 2A' IT/Z= in 96-Hr. lAbAE 4F - --- ?V!:;T\ -::z7v0-@W 6 malp, 10 ENVIRONMENTAL LABORATORY AQUATIC TOXICITY DATA SHEET DEFINITIVE (FULL-SCALE TEST) TYPE TESTO@o&, MATERIAL TESTEDW--I-PSF TEST ORGANISM r4tmm Mir-JNQIt)s I-ZSOS LC50's (95% CONFIDENCE LIMITS) PROBIT ANALYSIS T RUNS UN C, UN H TJRS -AB--HQITRq 72 HOURS 96 HOURS COMBINED 5SZ5 w--4Q 5 5 -,-w's sm :55clVKO (Ko L4mils)(@k Lim,-M) 554 (,4-2-Ot-52-cl @51ZW4 fl I (Kio 96 L7LOURS MOVING AVERAGE ANGLE METHOD @Slfl@ut@s 24 11OUItS 48 HOURS 72 HOURS 96 IIOURS .ui 'UN ,'4Sf ol COMBINED 96 HOURS ENVIRONMENTAL LABORATORY AOUATIC TOXICITY DATA SHEET EXPLORATORY (RANGE-FINDING TEST) LR Type Testlq6HR,_ la4C.UM :fsnkne_ Material Tested 05F (cc-1511l-q)LOtI- Test Organ ismFA-rrr=M_ tiiMkWtl)Source Date Recld. Batch No.l::B7 Avg. Wt. grams Avg. Size5,qCM No. Organisms p,-rdose - 5 Test Solution Volume 3 Liters/All-Glass Tank Tank Dimnsions:W IDE -MOUTH I GALLON GLASS J, Time Started I]: Date Started I 1q] B2j Date Complete d Dilution Water Carbon-filtered well water_(Temp. )C., 1).0. A.c9 Investigator (Full Signature -k L(: (95% Confidence Limits) so 12-Y&Zj PPM, PH-Bi-) Tank -!LO - Cl_ LM iA ZA Init: Conc miz/1 Totalt Anoun Added 24 Hours Total D.O. No. Dead pH PPM Control Ids 6 ....-... -to -- 10.0 48 Hours Total No.Dead pH D.O. pps 72 Hours Total H r.o. No.Dead ppm la-,1 Lv@l Hou@s Total No.Dead I )H 0 o A/ 1, 7 0 09Li2 0 Test Temp. C. zare-, Zj Oe7 Date Comments: UMUI MARK A&4EEg I-1011 f:)OLIIelcr- im ILVMEI@; Effects other than Mortality EC so l@r 4w :PRARY (=A?- Ewur 3RQQI,(IESfESM Tank No. Control Symptoms or Reactions 4kgb I-r 24-Hr. AEl-AIE I Total No. Affected 48 Hr. 72-Hr. f @.0 "-Hr. Ale 2A -All),uIAFI-D t'MMCItIS