Document Qg2d83mz8Exa02jLpea79YkvR

BIODEGRADATION (MANOMETRIC RESPIROMETRY -ANAEROBIC) TEST SUBSTANCE Identity:A mixturecontainingperfluorooctanesulfonatweh;i,ch may alsobe referredtoas PFOS, FC-95, or as a component ofFC-304 1. (1Octanesulfonicacid)(CAS # 2795-39-3). Remarks: The 3M productionlotnumber was not noted.The testsample is FC-3041. Currentinformationindicatesitisa mixtureof6% PFOS, 36% diethyleneglycolbutylether,36.05% water,12% Sultonefbamer,9% sodium octylsulfate0,.55% sodium laurylsulfatea,nd 0.4% tolyltriazole. The followingsummary applies to a mixture with incompletely charactoilzedconcentrations of impurities.Data may not accuratelyreflect the biodegradabilityof the tluorochomical component of the testsample. METHOD Method: Manometric RespirometryTest Test type: Anaerobic biodegradability GLP: No Year Completed: 1993 Analyticalmonitoring: Determinatioonfthemixtureratiofmethane and carbon dioxidereleasedinthe gas phase by gas chromatography,dissolved organiccarbon (DOC), and the releaseoffluoridbey fluoridseelectivelectrode and pH values. Statisticamlethods: Resultswere determined by calculatioonfthe percentage biodegradation. lnoculum source: Anaerobic sludge collectedfrom a community sewage treatmentplant(Lennestadt-Maumke,Germany) thatwas fed almostexclusively withresidentiawlastewater. Test condition: Dilutionwater: Not noted. Mineral NutrientMedium: MineralBasalMedium. Stock and testsolutionpreparation: Solutons ofthetestand reference materialswere prepared at100 mg C/L and 50 mg C/L, respectivelyw,ith mineralbasal medium. Testvessels: 118 mL serum flaskswhich containeda liquidphase volume of40 mL, closedwithbutylsepta and thegas phase purged with nitrogen. Incubator Conditions: Inthe dark. Temperature: 37 2 OC Agitation: None Number of concentrations: Test sample, testsample inhibiteds,odium benzoate (referencesubstance)and blankinoculum,allintriplicate. lnoculumconditioonn testinitiatio0n.:79g/Ldryweightpresenitn testsamples. Element Basis: Biologicamlineralizatiobny means ofthe releaseof methane and carbon dioxide. Test substance flaskconditions: pH: Not noted inthe report. RESULTS Nominal concentrations: Blank controlt,estmaterialat 100 mg C/L and sodium benzoate (referencesubstance)at50 mg C/L. Element values: 60-day % Degradationby Mineralizatio(nmethane and carbon dioxide)intestvessels7,8*,and 9 were 78.5,20.7 and 91 respectively. 60-day % Degradationby Determinationof DOC intest vessels7,8*,and 9 were 81.5,25.2 and 90.5 respectively. Fluoriderelease,by selectivfeluoridelectrodew,as not detectedinany ofthe testsamples (detectiolnimi2t pg F/L). *Could notconfirmwhat caused the low % degradationin thistestvessel. Remarks: Testingwas conducted on a mixtureas describedinthe Test Substance Remarks field.The values reportedapplytothatmixtureand notthe fluorochemicalproportionalone. CONCLUSIONS The testsubstance under anaerobicconditionswas categorizedas biologically degradable. The referencesubstance obtained89.5% degradationduringthe incubation periodof60 days as determinedby mineralizatio(n108% by DOC), thusthe validatiocnriterioafthe testwas fulfill(e>d60% degradationinsodium benzoate in60 days). Submifter: 3M Company, EnvironmentalLaboratory,P.O. Box 33331, St.Paul, Minnesota, 55133 DATA QUALITY ReliabilitKyJ:imischranking3. Lacks specificmethodology used and documentation. Sample puritywas not properlycharacterizedand the study lacksanalyticaclonfirmationofthe amount offluorochemicalproportioninthe solution. REFERENCES The studieswere conducted by FraunhoferInstitutfeorEnvironmentalChemistry and Ecotoxicology,D-57377 Schmallenberg,Germany atthe requestofthe FederalBureau forMaterialTechnology and Acquisibons,Gemiany, Grant No.: E/B31 E/PO078IN52275, 1993. OTHER Last changed: 6/26/00 FINAL REPORT ECO-TOXICOLOGICAL EFFECT OF FLUOR06SURFACTANIS Grant No.: EIB31EA?(W81NS275 Client Bundesamt fUrWaktechm-k und Beschaffung,Koblenz OWad Bureau forMaterialTechnologyand Acquisition@ InvestigatinIgnstitute: Fraunhoferinstitute forEnvironmentalChemistryand Eco-toxicology D-57377 Schmallenberg InstitutMeanager-* ProL Dr.W. Klein Projectleader.Dr.R. Debus Projectauthors: Dr.A. Fliedner Dr.K Hund DipL BioL R. N-iemann Dr. A. Remde December 1993 Trandator Andrea-losM Sdmekkr. 715-549-5734(C=man #1453/1995) Fmunhofer Institute forEnvironmentalChemistryand Eco-toxicology D-57377 Schmallenberg Investigatkmfor theEco-toxicologicaElvaluationoftheFluoro-surfactaBnatse FC-3041 Anurobic Degmdation Partg by Dr.A. Remde Mmsiaw. Andma-InVU Sdmeift,715-549-573(4G=m 8 #1453/1995) ANAER IC DEGRADATION Ile determinationof thebiologicaldegmdabilityof Base FC-3041 under anaerobic conditionswas done inthemanometric-respirometrytest(9). MATERL4L AND METHODS Test substance: Base FC-3041 (combinationof fluoro-surfactanitnsaqueous solution; Manufacuuer. 3M Company Germany, Neuss). Test criterion: Meammment of thebiological carbon dioxide. by means of thereleaseofmetham and Test method: A defmed volume (40ml) of an inoculatedmineral medium with a known concentrationof thetestsubstance(100 mgtl) isincubated'inthe dark in a closed serum flask(volume of 118 ml) at a constanttemperature(37*C 2).During the incubationperiodof 60 days thereleaseof medmw and carbon dioxideisdetermined by gas chromatography by extractingregularly0.5- I ml smples from thegasphase of the testnuL Test procedure: 15 testve&wls (serum fla with a volume of 118 mL of which 40 ml liquidphase) were preparedfor theperformance of thetest: Vessel 1,2 and 3: Vessel 4,5 and 6: Vessel 7, 8 and 9: mineralbasalmedium + inoculum mineral basalmedium + referencesubstance (sodium beawate 50 mg CIL) + inoculum mineralbasalmedium + testsubs== (100mg CIL) + inoculum (30 mg solidmauer/L) Trmgator An&ea-IngM Sdmeida,715-549-5734(Gmm 9 #145311995) VwwllO,Ilandl2: mineralbawl medium+ testsubstanc(e100mg CAL) + inoculum + mercurychloridesolution(0.001% final concenwation) The serum fla were closedwithbutylseptand thegasphase purged with nitrogen. Then the determinationof themetham and carbon dioxidecontentin thegas phase occurred.During the incubationperiodof 60 days at 37 2*C gas samples of 0.5- I ml were takenoutatregularintervalasnd themixtureratioofmethaneland carbon dioxidein thegas phase was determined.ne totalamount of the gases released(CCH4 and CC02) was determined through the addition of the concenuafionsof thegasesin the gas phase and thecalculatedconcentratioonf the gasesdissolvedin theliquidphase(10). 1"netotalamount of themineralizedcarbon(C.) ata certaintimeof measurement (t:=ni)scalculatefdrom thesum ofthereleaseofmetham (CCH4) and carbondioxide (CC02) inthedurationof incubatioonf60 days,followingtheequation(a). a) Cmm = I(CCH4)t-n- (CCH4)tmd + I(CC02)t-n- (CCa2)wd Ile bio-degmdationwas determinedaccordingtothefollowingequation(b): c b) Percentagebio-degradation Am x 100 CIS C.g. CTS = Totalamount of theminergizedcarboninmg C = Totalamount of thetestsubstanceused inmg C Additionallya,t thestartand end of the experimentst.he ph-value,thedissolved organiccarbon and thefluorideconcentratioinn the aqueous phase of the testruns were determined. Inoculum: An anaerobic sludge from a community sewage treatmentplant (LennestadtMaumke) which was fedalmostexclusivelwyith residentiwaalstewater,was usedas inoculum.The sludgewas thermostateduring the transporl4 ml sludgewere pipettedintothetestsamples,such thata dry weightof 0.79g/L was presentinthe testsample& lle samplecollectioonccurredon 9/28/1993. T=sWw. Andrea-lugMSdaidder,715-549-573(4Cvrnm #1453/1995) 10 Analysis: The determinatioonf the mixtureratioof methane and carbon dioxidein thegas phase was done ina Shimadzu 8A gas chromatographwith a thermalconductivity detectoroveraPorapak-N analyticasleparatiocnolumn.Ile analysisof thedissolved organiccarbonwas done in a TOC (TotalOrganicCarbon Analysis)500 of the Shimadzu Company. 1"nefluoridewas determinedby means of a fluorideselective electrod(eOrion69-90). Rderence substance:sodiumbenzoate(Merck,reagentgmde) Test period:9/30/1993- 11/29/1993 RESULIS During theincubationperiodof60 days,89.5% of thereferencesubstancesodium benzoatewas degraded(Tab.gl,Fig.gl).With that,thevaliditcyriterioonf thetest, a degmdationof sodium benzoate>60% in60 days,was fulfilled. lU degradatioonfBASE FC-3041 was verydifferenitntheduw = samplesstarted inparalletlo each other(Tab gl,Fig.g2).Accordingto themedmne and carbon dioxiderelease4, days afterstartintghe testa degradationof 10 - 13% could be observedin allthreevessels.In vessel9, the testsubstanceBASE FC-3041 was degradedata constantrateof degradationA.fter33 days,91% of thetestsubstance was mineralized. In thetestvessel7 thetestsubstanceBASE FC-3041 did atfirsntot furtherdegrade from day 4 to day 25.Only after33 dayscould a sigafficandtegradationbe observed again.Afteran incubationperiodof 60 days@a degradationof 78.5% was achieved. Paralletlo vessel7,thetestsubstanceBASE FC-3041 invessel8 did atfirstnot furtherdegradefrom day 4 today 25.Here too, a restaritndegmdation couldbe observedafter33 days,however, with a substantiallyower rateof degradationin comparisontovessel84.After60 days,only 20.7% of thetestsubstancehad degraded inthistestsample. 4giC.must be -r. Tmuslatw.Andma-IngriSd meWer,715-549-573(4G=m #1453/1995) The causeforthisdegradativbeehaviorin thetestvessels7 and 8 isnot known. IU possibilietxyiststhatduringthe sample collectioonr duringincubationoxygen diffusedin variousamounts intothe testsamples,through which the anaerobic mineralizatiownas inhibitetdodifferendtegrees.A confumiaory testforoxygen in thevessels7 and 8 witha.suitablceolorindicato(rresazurinw)as not possibledue to thedark blackcoloratioonfthe testsamples.However, the differendtegradationof BASE FC-3041 observedin thetestsamples may alsobe u=d to the inoculum. Sludgerepresentas verycomplex inoculum witha largediversityN.ot allorganisms are capableof degradingthe testsubstanceto the same extenl Therefore,the possibiliteyxiststhata differendtistributiofnvariousorganismsin thetestvessels occurredduringthe additionof the inoculum,which led to the differencien degradationof the testsubstanceobserved. Tab.g2 shows the resultsof the determinationof the anaerobicdegradationof BASE FC-3041 by means of themineralizatiotnomethane and carbon dioxidein comparisontothedeterminatioonf thedecreaseof dissolvedorganiccarbon.A very good agreementbetween thetwo methods was found in alltestsamplesforthe test substanceaswell asforthereferencesubstance. A releaseoffluoridbey means of a selectivfeluoridelectrode(detectiolnimit2 gg fluoride)'wansot detectablienany ofthetestsamples.During the mineralizatioonf fluorinatecdompounds, fluodw can inprinciplbee releasedonly asfluorideion.A volatilizatioofnfluoridew,hich isobservedforlow ph-values,can be excludedunder the given slightlaylkalineconditionsm,easured at the startand the end of the experimenllle possibilietxyiststhatreleasedfluoridewas bonded to the glass vesselsorto theorganisms. EVAILUATION Based on the present testresults,the test substance BASE FC-3041 may be categorizedas biologicalldyegmdable under anaerobicconditions. TmnWw. Andrea-InVW Schndder, 715-549-5734 (Gmm 12 #1453/1995) Tab. gl: 'IneralizatoifoBnASE FC-3041 underanaerobicconditions Day Inoculum Referencesubstance Caln I) Gain Z Xdevmiation ag c at C Base FC-3041 + HgCI2 CaLin 1 ag C 0 0 0 0 4 0,279 0 0 11 0,703 0 0 25 1,206 0*4 20 33 lt343 1,337 6608 so 19392 1-9709 8995 0 nb nb nb 0,04 0106 Day 0 4 11 25 33 60 Test Substa=e Vessel 7 Cain 31 mg C Use FC-3MI Vessel 8 %degradation CMin 3) ag c Vessel 9 degradationCain 2 ag C % degridition 0 09428 0,394 09442 11913 3,141 0 1097 9,8 itil 47.2 7895 0 Os534 0,533 09407 0.612 0,831 0 1393 13,3 1092 is.l 20,7 0 Ol48l 1,657 39412 3.641 0 12 l: 41,! 91 1) Average value from 3 runs 2) Average value from 3 expenmentid runs mmus Cmm of the moculum 3) Cmin of the experimenml mmus Cmin of the inoculum control control nb = not dewxmined TruLdatw.Andma-IngM Sdmeida,715-549-573(4Gaman #1453/1995) 13 Tab. g2: Tictermirmtioonf theanaerobicdegradationofBASE FC-3041 and sodium benzoate by means of minemfiizaai-iaon-dnmeasurement of the dissolved organiccarbon(DOC) Na - benzoate 1) in % degmdation 9905 of theDOC % degradation 105 BASE FC-3041 Vessel 7 Vessel 8 Vesse]L 9 7895 2097 8195 2592 20,$ 1)Avmge valuefrom 3 p=W [runs] Tmsluw. Andma-hWW Sdmdder 715-549-5734(Omm 14 #145311995) ,Figg.l:Anaerobicdegmdationof sodium benzoate(averagevaluefrom 3 paralle[lruns]) 100 2 Degradation 80 60- 40- 20- OC9 s s 0 10 20. 30 40 so 60 70 DAYS Trandator Andrea-InVM Schneida,715-549-5734(German #1453/1995) 15 Fig.g2:AnaerobicdegradationofBASE FC-3041 in3 paralleslamples Z Degradation 100 so- 80- 40- 20 0 10 20 30- 40 -50 00 70 DAYS Vessel 7 Vessel 8 Vessel 9 Trandatw. Andma-InSM Sdmdder, 715-549-5734(Gmm 16 #145YI995)