Document e17YN9Yz7DjmN7j8ddx8zZEx9

AR 226 - 0900 BIODEGRADATION (MANOMETRIC RESPIROMETRY -- ANAEROBIC) TESTSuBsTANCE Identity: ArefmeirxrteudretocaonstPaiFnOiSng, pFeCr-f9iu5o,rooorcatasneasuclofmopnioantee;n,twohfiFcCh-m30a4y1.als(o1-be Octanesulfonic acid) (CAS # 2795-39-3). Remarks: FC-3041. CurTrheent3iMnfporrmoadtuicotnioinndlioctantuesmbiteirs waamsixntoutrenootfed6.% TPhFeOSte,st3s6a%mple is doicteytlhysluelfnaeteg,ly0c.ol56bu%tysloedtihuemr,la3u6ry.l05su%lfwaattee,ra,n1d20%.4S%ulttoolnyletifaozaomleer., 9% sodium tcThhheaerbafiocoltdleeorgwirizanedgdabcsioulnmictmeyanotrrfyattahipeopfnllisoueofsrtoiocmpahuemrmiiitxcitaeuslr.ceoDwmaiptthoanrimenacnoytmonpfolttehtaeeclctyuersattsealmyprleef.lect METHOD TMeestthotdyp:e:MaAnnoameertorbiicc RbeisodpeigrroamdeatbrilyiTtyest GLP: No AYneaalrytCiocmapllmeotneidt:ori1n9g9:3 carbon dioxide released Deter in the mina gas tionofthe phase by g amisxctuhrreomraattioogorfapmheyt,hadinsesoalnvded organic carbon (DOC), and the release of fluoride by fluoride selective electrode SatnadtipsHticvaallumees.thods: Results were determined by calculation of the percentage tbIirnoeodacetgumrleanudtmatpsilooaunn.rtc(eL:enAnneasetraodbti-cMasulmukdeg,e collected f Germany) rtohamtawacosmfmeudnailtmyossteweaxcgleus iv e ly with residential wastewater. Test condition: MDSiitlnouectrkiaolanNnwudattrteeirse:tntsNoMoletudtniiooutnemd:p.reMpianreartailonB:asaSlolMuetidoinusmo.fthe test and reference materials were prepared at 100 mg C/L and 50 mg CIL, respectively, with Tmiensetravlesbsaeslasl:me1d1i8umm.L serum flasks which contained a liquid phase vniotlruomgeen.of 40 mL, closed with butyl septa and the gas phase purged with IncubaTteomrpCeornadtiutrieo:ns:37In2theCdark. NumbeArgiotfactioonnc:entNroanteions: Test sample, test sample inibited, sodium benzoate (reference substance) and blank inoculum, all in triplicate. 002885 Inoculum condition on test initiation: 0.79 g/L dry weight present in test samples. Element Basis: Biological mineralization by meansofthe release of Tmeestthasnuebsatnadnccaerfbloanskdicooxinddei.tions: pH: Not noted in the report. RESULTS sNoodmiiunmalbecnoznocaetnetr(arteifoenresn:ceBsluabnsktcaonnctero)l,atte5s0t material mg CL. at 100 mg C/L and Element values: c6a0r-dbaoyn %dioDxeidger)adianttieostn vbeyssMeilnesr7a,li8za,taionnd(9mweethraen7e8.a5n,d20.7 and 91 60-day respectively. % Degradation by Determination of DOC in test vFelsuosreildse7r,e8le,asaen,db9ywseerleect8i1v.e5,fl2u5or.i2deanedlec9t0r.o5der,eswpaecstinvoetly. d"eCtoeucltdendoitncaonnyfoifrmthwehattesctasuasmepdltehse(ldoewt%ectidoengmraida2ttioping iFn/L). this test vessel. Remarks: `Substance Testing was conducted on Remarks field. The values arempioxrttuerdeaapspldyestcortihbaetdmiinxttuhreeTaensdt not the fluorochemical proportion alone. CONCLUSIONS Thetest substance under anaerobic conditions was categorized as biologically degradable. Tpehreiordeoffer6e0ncdeasyusbasstadnecteerombitaniendebdy8m9i.n5er%adliezgartaidoanti(o1n08du%ribnygDtOhCe)i,nctuhbuastitohne validation criteriaofthe test was fulfilled (>60% degradation in sodium benzoate in 60 days). Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 DATA QUALITY dReolciuabmielnittya:tioKni.imiSscahmpralnekipnugri3t.y wLaascknsotsppercoipfeirclmyecthhaordaoctleorgiyzeudseadndantdhe study lacks analytical confirmationofthe amount of fluorochemical proportion in the. solution. REFERENCES 00288 Tahnde sEtcuodtioexsicwoelrogeyc,oDn-d5u7c3t7e7d bSychFmraalulnehnobfeerrg,InGsteirtumtae nfoyar tEntvhierornemqeunetsatlofChtehmeistry Federal Bureau for Material Technology and Acquisitions, Germany, Grant No.: E/B31E/PO078/N52275, 1993. OTHER Last changed: 6/26/00 002887 Co Fe-%04L FINAL REPORT ECO-TOXICOLOGICAL EFFECT OF FLUORO-SURFACTANTS Grant No: E/B31E/POOTS/NS27S Client: `Bunfdiie rWesrktaecmhnt ikund Beschaffung, Koblenz - (Bederal Bureau for Material Technologyand Acquisition) Investigating Institute: Fraunhofer Institute. for Environmental 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 7 Dipl. Biol. R. Niemann Dr. A. Remde December 1993 "Transistor: Andrea-Ingrid Schneider, 715-549-5734(German#1453/1995) 00288E Fraunhofer Institute for EnvirCheomisntrymaned Ecno-ttoxiacololgy D-57377 Schmallenberg Investigatfionr theEco-tEvoaluaxtioi nofctheFoluorlo-so urfugctanitBac seFaC-3l041 AnaerobicDegradation Partg by Dr. A Remde 8 Translator: Andrea-IngridSchmelder,715-549-5734 (German#1453/1995) 002889 ANAEROBIC DEGRADATION Thedeteroftmheibiolnogiacaltdegriadaobilnityof BaseFC-un3der0ana4ero1bic `conditionswas doneinthemanometric-respirotemsett(9r)y. MATEANRDMIETAHOLDS `Testsubstance: Base FC-3041 (combofiflunoroa-sutrfaictaontsninaqueoussolution; `Manufacturer: 3M Company Germany, Neuss). `Testcriterion: Measurementofthebiological mineralization bymeansofthereleaseofmethaneand carbon dioxide. `Testmethod: A defined volume (40ml) of an inoculated mineral medium with a known conceonfttherteasttsubistoannce (100mg/L)isincubatedinthedarkin aclosed serumflask (volume of 118 ml)at aconstant temperature (37+2)C.Duringthe incubationperiodof60 daysthereleaseofmethane and carbondioxideisdetermined bygaschromatographybyextractingregularly 0.5 - 1mlsamplesfromthegasphase ofthe testrun. - Test procedure: 15testvessels (serumflaskswith avolumeof 118ml,ofwhich40mlliquidphase) werepreparedfor theperforomfathnetceset: Vessel1,2and3: mineralbasalmedium +inoculum Vessel 4,5and 6: mineralbasalmedium +referencesubstance (sodiumbenzoate50mgC/L) +inoculum - Vessel7,8and9: mineralbasalmedium +testsubstance (100mgC/L) +ino(3c0mgusollidmautterm/L) "Translator: Andrea-Ingrid Schneider, 715-549-5734 (German #1453/1995) 9 002890 Ve1s0,s11aend1l2: mineralbasalmedium +testsubstance (100mgC/L) + inoculum +mercurychloride solution (0.001% final concentration) Theserumflaskswereclosedwithbutylseptaandthegas phasepurgedwithnitrogen. Thenthe determinationofthemethane and carbon dioxide contentinthe gas phase occurred. During the incubation period of60days at 372C gas samples of 0.5- 1mlweretakenoutatregularintervalsandthemixtureratioofmethaneand carbondioxideinthegas phasewasdetermined. Thetotal amountofthegases released (CCH, and CCO,) was determined through the addition of the concentrationsofthe gasesinthegasphaseandthecalculatedconcentrationofthe gasesdissolvedintheliquidphase (10). Thetotalamountof the mineralized carbon(Cia)at 8certaintime of measurement (t=n)iscalculatedfromthesum ofthereleaseofmethane (CCH)andcarbondioxide (CCO;)inthedurationofincubatoifo60n days, following the equation (a). 2) Caio = [(Cartelien - Cazaadena] + (Cooma - (Cool Thebio-degradation wasdeterminedaccording to the following equation (b): b Peeragetioegradaion= x100 Cun =Totalamountofthemineralizedcarbonin mg C Crs =Totalamountofthetestsubstanceusedinmg C Additionally, at the start and end of the experiments the pH-value, the dissolved organiccarbonandthefluoride concentrationintheaqueous phaseofthetest runs `were determined. Inoculum: An anaerobic sludge from a community sewage treatment plant (Leanestadt'Maumke) whichwasfedalmostexclusivelywithresidential wastewater,wasused as inoculum, The sludge was thermostated during the transport. 4ml sludge were pipettedintothetestsamples, suchthat adry weight of 0.79g/L waspreseatinthe test samples. The sample collection occurred on 9/28/1993. Transistor: Andres IngridSchneider,715-549-5734(German 14531995) 10 002891 Analysis: * Thedeterminationofthemixtureratioofmethane andcarbondioxideinthegas phasewasdonein a Shimadzu8Agas chromatograph with athermalconductivity detectorover aPorapak-Nanalyticalseparationcolumn.Theanalysisofthedissolved organic carbon was done in aTOC (Total Organic Carbon Analysis) 500ofthe `Shimadzu Company. The fluoride was determined by meansof a fluoride selective. electrode (Orion69-90). Referencesubstance:sodiumbenzoate(Merck,reageatgrade) Testperiod: 9/30/1993 - 11/29/1993 - RESULTS Dutrheiincunbatgion peorfi60odayds, 89.5%ofthereference substance sodium benzoate was degraded (Tab. g1, Fig. g1). With that, the validity criterionofthe test, adegradationofsodium benzoate>60%in60days,wasfulfilled. Thedegradationof BASEFC-3041wasverydifferentinthethreetestsamplesstarted in parallel to each other (Tab g1, Fig. g2). According to the methane and carbon dioxiderelease, 4days afterstartingthetest adegradationof10- 13%couldbe observed in all three vessels. In vessel 9, the test substance BASE FC-3041 was. degradedat aconstantrateofdegradation.After 33days, 91%ofthetestsubstance wasmineralized. Inthetestvessel 7thetetsubstance BASEFC-3041didatfirstnotfurtherdegrade. from day 4today25.Onlyafer33dayscould asignificantdegradationbe observed again.Afteranincubationperiodof60days,adegradationof 78.5%wasachieved. `Paralleltovessel7,thetestsubstance BASEFC-3041 in vesse8l didatfirstnot furtherdegradefromday 4today 25.Here 00, arestartindegradacotuildobne observedafter 33 days, however,with asubstantiallylowerrateofdegradatiionn comparisontovessel84.After60days,only20.7%ofthe testsubstancehaddegraded inthistestsample. -- sic.Mustbe 7. ' "Translator: Andrea-IngridSchneider, 715-549-5734(German #1453/1995) 11 002892 "The causeforthisdegradativebehaviorinthetestvessels 7and 8isnotknown.The `possibility exists that during the sample collection or during incubation oxygen diffused in various amounts into the test samples, through which the anaerobic `mineralizationwasinhibitedtodifferentdegrees. Aconfirmatorytestforoxygenin thevessels 7and 8with suitablecolorindicator (resazurin) wasnotpossibledue thedarkblackcolorationofthetest samples.However,thedifferentdegradationof BASEFC-3041 observed in thetestsamples may also be traced to the inoculum. Sludgerepreavsereycnomtplesxinoculumwith alargediversity. Not allorganisms are capable of degrading the test substance to the same extent. Therefore, the possibilityexiststhata differentdistribution ofvariousorganismsinthetestvessels occurredduringtheadditionof theinoculum, whichledto thedifferencein degradation ofthe testsubstance observed. . - Tab. g2 shows the results of the determination of the anaerobic degradation of BASEFC-3041 by meansofthe mineralization to methane and carbon dioxide in comparisontothedeterminationofthedecreaseofdissolvedorganiccarbon. Avery goodagreementbetweenthetwo methods was foundinalltestsamplesforthetest `substanceaswellasfor thereferencesubstance. Areleaseof fluoridebymeansof aselectivefluorideclectrode (detectionlimit 2jg fluoride) wasnotdetectableinanyof thetestsamples.Duringthemineralizationof fluorinatedcompounds, fluorinecaninprinciplebereleasedonlyasfluorideion. A volatilizationof fluoride,whichisobservedforlow pH-values,canbeexcludedunder the given slightly alkaline conditions, measured at the start and the end of the experiment. The possibility exists that released fluoride was bonded to the glass vesselsor 10 the organisms. EVALUATION : Based on the present test results, the test substance BASE FC-3041 may be categorized as biologically degradable under `anaerobic conditions. Translator: Andrea-Ingrid Schneider,715-549-5734 (German #1453/1995) 12 002893 Tab. g1:Mineralizationof BASEFC-3041underanaerobicconditions --- Day Inoculum Referencesubstance --_-- cminng 1) Cainng 2) Xdegradation 0 0 4 0,219 n 0,703 25 1,208 0,4 20 33 1,343 1,337 66,8 6 1,302 1,789 29,8 _ Base FC-3041 + HgCly Cminng C1) nb nb ab 0,08 0,08 _ nd 0 4 1 aF Cain 3) og C '0 0,428 0,394 BeTEI 8 degradation Cain =g C3) 0 10,7 0,534 9.8 0,533 Vesser 9 degradation Cain ng 3) 0 0 13,3 0,481 13,3 1,887 xgeaxiiidac 0 12,0 at 23 0,442 11,1 0,407 10,2 3,42 85,: 33 1,013 47,9 0,612 15,3 3,841 a 60 3,141 18,8 0,831 20,7 -- 21)Avveeranggevaaluefrroomm 3exppeerriimmeennttaallrruanssminsCinoftheinoculum control - 3) Cain ofthe `unsminusCinoftheinoculumcontrol nb =notdetermined 1B "Translator: Andrea-Ingrid Schneider, 715-549-5734(German #1453/1995) 00289 Tab. g2: DbeetnezromaitneatbiyomnoefatnhseoafnameinreorbailcidzeagtriaodnatainodnomfeaBsAurSeEmFeCn-t3o0f4t1haenddisssoodlivuemd organiccarbon(DOC) -- Wm% adeglramdaitiomn Deem%mdSeegorladeaDtOiCon Ha - benzoate 1) 89,5 108 BASE FC-3041 Vessel 7 8,5 Vessel 8 20,7 . Vessel 9 1 1) Averagevaluefrom 3parallel [runs] 81,5 25,2 90,5 1" "Translator: Andrea-Ingrid Schneider, 715-549-5734(German #1453/1995) wUR89S mp Fig. 1:Anaerobic degradationofsodiumbenzoate (averagevaluefrom 3parallel [runs]) | | so}1 || I j wl | | | :/! i| 20 C/d | / heol Qos ] 0 10 20 30 40 50 60 70 Translator: Andrea-IngridScheider,715-549-5734 (German#1453/1995) 15 002856 Fig. g2:Anaerobic degradation of BASEFC-3041 in 3parallelsamples 100 Liummmiation 80 F / o / | 80 /' ` 40 7/ 20 ! | . | i 1 20 30.oars 40 6S 80 70 ~~ Vessel 7 --S-- Vessel 8 --8-- Vessel 9 "Translator: Andrea-Ingrid Schneider, 715-549-5734(German #1453/1995) 16 00289