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AR 226 - 0297 BIODEGRADATION (MANOMETRIC RESPIROMETRY -- AEROBIC) TEST SUBSTANCE Identity: A mixture containing perfluorooctanesulfonate, which may also be referred to as PFOS, FC-95, or as a component of FC-3041. (1Octanesulfonic acid) (CAS # 2795-39-3). Remarks: The 3M production lot number was not noted. The test sample is FC-3041. Curent information indicates it is a mixture of 6% PFOS,36% diethylene glycol butyl ether, 36.05% water, 12% Sultone foamer, 9% sodium octyl sulfate, 0.55% sodium lauryl sulfate, and 0.4% tolyltriazole. The following summary applies to a mixture with incompletely characterized concentrations of impurities. Data may not accurately reflect the biodegradability of the fluorochemical component of thetest sample. METHOD Method: Manometric Respirometry Test Test type: Ready biodegradability GLP: No `Year Completed: 1993 Analytical monitoring: Oxygen consumption determined by measurement of the amount of oxygen generated electrolyticaltloy maintain a constant gas volume in the respiration flask. Depletionof dissolved oxygen was registered automatically. Amountof oxygen taken up is given (after comparison with the blank inoculum) as a percentageofthe chemical oxygen demand. Statistical methods: Results were determined by calculationofthe percentage biodegradation. Inoculum source: Activated sludge collected from a community sewage plant (Schmallenberg, Germany) that was fed almostexclusivelywith residential wastewater. Test condition: Dilution water: Not noted. Mineral nutrient medium: Mineral Basal Medium Stock and test solution preparation: Solutions of the test and reference materials were prepared at 100 mg/L with mineral basal medium. Test vessels: Closed flasks kept at a constant temperature. Each vessel is connected gastighttothe pressure regulator corresponding to it. Incubation Conditions: Per manometric method - Temperature: 22+2C Agitation: Continuous stirring Number of concentrations: Test sample, test sample inhibited, test `sample plus aniline, aniline (reference substance) and blank inoculum, all in duplicate. 002875 Inoculum condition ontestinitiation: Initial solids 3 g/L, 30 mg solid mEaltetemre/nLt. Basis: Biological degradation by meansofoxygen Tcoensstusmupbtisotna,ncmegfOlaLs.k conditions: pH: Not noted. D.O.: Automatically measured. RESULTS --- Nominal concentrations: Blank control, test material at 100 mg/L, and aniline (reference substance) at 100 mg/L. Element values: a1v4e-rdaaygeDeofgrtawdoatriepolnicwaittehsTmeisntuMsattehreiablla=nk9.3.8% based on b1a4s-deadyoDnegarvaedraatgieoonfwtiwtoh TreepslticMaatteesrimailnpulsusthAeniblliannek.= 88% b1a4-sdeadyoDnegarvaedraatgieonofwtitwho TreesplticMaatteesrimailnIunshitbhietebdla=nk8..5% Remarks: Substance Testing was conducted on Remarks field. The values a mixture reported as described in the Test apply to that mixture and not the fluorochemical proportion alone. ONCLUSIONS ----- Tohxyegteenstcmoantseurmiaplti%ondoefgrtahdeabtliaonnkbcaosnetdroolnwathse9m3e.a8n%oaffttewro14redpalyisc.ates minus the vTahleidrateifoenrecnrciteersiuobnostfatnhceeteosbttwaiansedfu8lf2il%ledde(g>ra6d0a%tiaoftnebry1414dadyasy)s., Tthhuesttehset was terminated on day 14 since the validity criterionofthetestwas fulfiled and the oxygen uptake reached a plateau. Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 ATA QUALITY --_ dReolciuambeilnttya:tiKoini.misScahmpralnekipnugri3t.y wLaascknsotsppercoipfeirclmyecthhaordaoctleorgiyzeudseadndanthde study lacks analytical confirmationofthe amountof fluorochemical proportion in the solution. nee REFERENCES This study was conducted by Fraunhofer Institute for Environmental Chemistry and Ecotoxicology, D-57377 Schmallenberg, Germany at the request of the 002876 Federal Bureau for Material Technology and Acquisitions, Germany, Grant No. E/B31E/PO078/N52275, 1993. OTHER s-- r -- Last changed: 6/26/00 002877 . Fe-%041 FINAL REPORT ECO-TOXICOLOGICAL EFFECT OF FLUORO-SURFACTANTS Grant No: E/B31E/POOTS/NS275 Client: `BunfdireWesrka tecmhntik und Beschaffung, Koblenz - (Federal BureanforMaterial Technology and Acquisition): Investigating Institute: Fraunhofer Institute. forEnvironmental Chemistry and Eco-toxicology D-57377 Schmallenberg Institute Manager: Prof. Dr. W. Klein `Project leader: Dr. R. Debus Project authors: Dr. A. Fliedner Dr. K. Hund Dipl. Biol. R. Niemann Dr. A. Remde. December 1993 "Translator: Andrea-IngridSchneider,715-549-5734(German#1453/1995) 002878 Fraunhofer Institute for EnvirCheomisntrymaned Ecno-ttoxiacollogy D-57377 Schmallenberg Investigation for the Eco-toxicological EvaloftuheFaluotro-siurfoactnant Base FC-3041 Aerobic Degradation Partf by Dr. A. Remde Translator: AndreaIngridSchneider,715-549-5734 (German #1453/1995) 2 002879 AEROBIC DEGRADATION The determinationoftheeasy biologicaldegradofaBabseiFlC-t304y1underacrobic `conditionswas doneinthe manometric-respirtoesmte(r8)y. MATE ANR DMI ETA HOL DS `Testsubstance: `Base FC-3041 (combinationoffluoro-surfactanitns aqueous solution; Manufacturer: 3M Company Germany, Neuss). Testcriterion: Measurementofthebiological degradability by meofathen oxygsen consumption. Testmethod: Adefinedvolumeofaninoculatedmineralmediumwith aknownconcentration of thetestsubstance (100mg/L)isstirredin aclosed flaskat aconstanttemperature (22C +2).The oxygen consumptionis determinedthroughthemeasurementofthe. amount of oxygen generated electrolytically that is necessary to maintain a constant gas volumeintherespirationflask.Thegenerated carbon dioxideisabsorbedinto 8 solution of potassium hydroxide. The amount of oxygen taken up by the test substanceisgiven (afterconsideringthecorresponding valueintheinoculum blank testperformedinparallel)aspercentageof the CSB!(chemicaloxygendemand). Testprocedure: 10testvessels were preparedfor theperformanceofthetest: Vessel 1and 2: mineralbasalmedium +inoculum Vessel3and 4: mineralbasalmedium +referencesubstance (100 mg/L) +inoculum(30 mgsolid matter/L) sme VinEnglish:COD. 1willpreservethe German abbreviationssince they arepresentinformulasandtables. "Translator: Andrea-Ingrid Schneider, 715-549-5734(German #1453/1995) 3 002880 Vessel Sand 6: mineralbasalmedium +testsubst(1a00nmgc/eL) +ino(3c 0mgusoll idmautterm/L) Vessel 7and 8: mineralbasalmedium+referencesubstance (100 mg/L) + test substance (100 mg/L)+ inoculum (30 mg solid matter/L) `Ve9sasnde1l0: mineralbasalmedium +testsubst (1a00nmgc/eL) +inoculum (30mgsolid matter/L) +mercury chloride solution (0f.ina0lcon0cent1rati%on) The vessels wereclosedandplacedintotherespirometer.Aftertemperatureand pressurecompensation (approx.0.5hours),eachvessel wasconnectedgastighttothe: pressureregulatorbelongingtoit. Duringthetestperiodthedepletionofdissolved oxygenwasregisteredautomatically. - Thebio-degradation was determined accordingtothefollowingequation: Perceatagebi.o-degradation =._G(Br SB-oB)tx1e00 BSB =biochemicaloxygenconsumptionofthetestsubstance (mg) B= depletionofdissolvedoxygenofthebasalmediumwithinoculum (mg) CSB =chemical oxygenconsumpti(omng?) | ThSB =theoorxygeentdeimacnda(mlg) Inoculum: Active sludge from acommunity sewagetreatmentplant (Schmalleaberg) whichwas fedalmostexclusivelywithresidential wastewater, wasusedasinoculum.Theactive sludge was aerated during the transport. The inoculum was adjusted with isotonic Ringer'ssolutionto 2solidscontentof 3g/L andaerated.Thesamplecollection occoun1r0/r28/e199d3. {hiinstchaeseetxhtesabaomveea,bCbSrBevwiaasticohneCmSiBshiesruSsaesdefrosrtcohfeemdiasccfh,ewrhSicah uGaensrlisesiocfhevmwiehciarclhobxtyrrgaanelnasdieecms0ahnd.Ia cheoxym geni conc suma ptil on. Translator: Andres-Ingrid Schneider, 715-545-5734(German #1453195) 4 002881 Analysis: To determine the dissolved oxygen depletion, a sapromate of the Voith Company (Heidenheim) was used. The oxygen consumption was automatically registered as BSBIL. Reference substance: aniline (Merck, reagent grade) Test period: 10/29/1993 - 11/12/1993 RESULTS `The results arereprienTsab.e1nantdFieg.fdl. Duringtheincubationperiodof14days,82%ofthereference substanceaniline was degraded.The validitycriteriaofthetest (degradationofaniline >40% af7tdeayrs and >60% after 14 days) were fulfilled. 93.8% ofthetestsubstanceBaseFC-3041 wasdegradedinthesameperiodoftime. Sincealready88.6%ofthesubstancehaddegradedwithin 10dayscountedfrom the day the degradation for the first time surpassed 10%, the substance may be categorized as easily biologically degradable. Thetestcouldbetermionnedady14since all validity criteriaof thetesthadbeen fulfilledand aplateauwasreachedfor theoxygenuptake. EVALUATION Based onthepresent results,thetestsubstanceBaseFC-3041wascategorizaeds easily biologically degradable. Translator; Aodrea-lngridScheider,715-549-5734 (German #1431995) 5 002882 Table 1: BSSBB and %ofbiologicaldegradationof thetestsubstanceFC-3041andofthereference TeStsatrtsoufbstthaentceest(:TS): TCehsetmciocnaclenotxryagtieonnc:onsumption (CSB): B1a0s2e9/F1C9-933041 100308mmgp//Lmg subsiance Reference substance(RS): TInoocruliuimcopen consumption (ThSB;(ThSB; Nis) Tie 2p A t famrggsysubstance Dap Docalm Referencesbsizos "Testsubsiance RS+TS T+HSCl saBg l02)/1 8g 02T/1ue)Zdcgratation ug 0T2/B1SB%3)degradatoiTon mg 02E/S]B3Xi)cgratstson TngB02/41) z 19u8 00,,00 0000 1101,,50 m19s.3 1104.80 3n.e0 23.00 13 2018800 114,80 0640 3224,05 235,s6 13732.00 1802,,03 34,00 56 2.2085 1541.s0 2m3,s1 5ee3s0 6705,.26 225368.,50 728,,30 55.00 87 a2800 e17s5s5 @721,8 17400 880.,17 227626,.08 s82n,o7 6500 19003209,55 118884.08 786.23 116.05 886,,69 227861.05 88,.04 61.00 a12 t3250 L14s8 8709,,75 8791.05 9s02..30 28814,.00 8a6.23 11.00 W13334055 1w6n.s0 8812,,30 8B2.s5 9933..88 228899.55 8888,,00 8B.850 12))IAnvoecurlaugme cvoanluteroflrom two expeimenal runs, minus the oxygen cousumption by the inoculum c3o)nAtvreorage valuefrom two experimenrtunasl, mitnhGuxygsen consumpbtyitohn inoculum 4c)oTnestsubstancewithinoculumandHgCl,solution, averagevaluefrom twoexperimentraunls T3a1agtwhheiocrhgirnaalmnilya#1dvyi.sble By analogy to table 1 on page 6,thebeadingofthiscolumnmustbe Translator: Andre-IngedSchneider, 71S-549-5T34(German #1453/1995) 6 002883 100LZ sEmdarton ' Fig. fl: Biologicaldegradation,of se se substance BASE eX andofthe ----9 80 = it 60 [7 L : - 40 Jf] 17 | g 20 va , 0 Fst - 0123 45o6 a 78 . 9 MH11 2180 14 = 18 RS > Base FC-3041(TS) --%= Aniline(RS) "Translator: Andrea-IngridSchneider, 715-549-5734(German#1453/1995) 7 002884