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ACTIVATED SLUDGE RESPIRATION INHIBITION TEST TEST SUBSTANCE Identity:Mixturecontainingperfluorooctanesulfonawtheich may also be referredto as PFOS, FC-95, or as a component ofFC-3003. (1Octanesulfonicacid)(CAS # 2795-39-3). Remarks: The 3M productionlotnumber was notgiven.The testsample isFC-3003. Currentinformationindicatesitisa mixtureof1% PFOS, 15% diethyleneglycolbutylether,79.39% water,2% Sultonefoamer, 1.5% sodium octylsulfate,1% sodium decylsulfate0,.06% sodium laurylsulfatea,nd 0.05% benzotriazole. The followingsummaty applies to a mixture with incompletely characterized concentrations of impurities.Data may not accurately reflecttoxicityof the fluorochemical component of the testsample. METHOD Method: OECD Guideline209 GLP: No Year Completed: 1997 Analyticalmonitoring: Dissolvedoxygen concentrationtse,mperature,and pH. Statisticalmethods: Resultswere determined by calculationof the % inhibitioinn respiratiornate. Test organism source: Activatedsludge mixed liquorcollectedfrom the Metro Wastewater Treatment Plant,St.Paul,MN. Test condition: Dilutionwater: Carbon-filterewdellwater (3M well#2, St.Paul,MN) Syntheticsewage: per OECD method Reference and testsolutionpreparation: A stocksolutionofthe referencesubstance,3,5-dichlorophenowla,s prepared by dissolving 500 mg in 1OmL 1N NAOH, dilutedto 30mL withMilliporMeilli_QTM water,then broughttothe pointofincipienptrecipitatiownithIN H2SO4 and dilutedto 1L withMiili_QTM water. The pH ofthe referencesolution was measured to be 6.3.Test substancewas added directltyothe testvessels. Test vessels: Not given. Number of concentrations: fiveplusblankcontrol Temperature: 19.2- 21.60C Totalsuspended solidsand pH on day of testing:4.04 g/L (TSS in final1.61g/L),initipaHl 7.9and finalpH 8.6 Element Basis: Respirationinhibitiaosn determinedby oxygen consumption. Remarks: Values correctedto200C forcalculations. RESULTS Nominal concentrations: Blank control,10,50, 100, 500,and 1000 mg/L. The blankcontroland 1000 mg/L were duplicated Elementvalues: 30-minuteEC50=>1000mg/L 3-hour EC50 = > 1000 mg/L Element valuesbased on nominal concentrations. Remarks: Testingwas conducted on the mixtureas describedinthe Test Substance Remarks field.The valuesreportedapplytothatmixtureand not the fluorochemicalproportionalone. CONCLUSIONS The testsubstance 3-hourECro foractivatedsludge respiratioinnhibitiownas determined tobe >1000 mg/L. Thisconcentrationinhibiterdespiratiobny -24%. Submitter: 3M Company, EnvironmentalLaboratory,P.O.Box 33331, St. Paul,Minnesota,55133 DATA QUALITY - - ReliabilityK:limischranking= 2. The studymeets allthecriterifaorquality testing.However, sample puritywas not propedy characterizedand the study lacksanalyticaclonfirmatioonfthe amount offluorochemicalproportioninthe solution. REFERENCES Thisstudywas conducted by the 3M Company, EnvironmentalLaboratory, St.Paul,MN, Lab Request number R1331, 1997. OTHER Last changed: 6/26/00 ENVIRONMENTAL LABORATORY AC-NVATED SLUDGE MIXED UQUOR Date 3 -,;1-19-7 Analyst 'TW-c-7 Page I of Type Test OC-c-0 AC-TIVA-T-CD @5LUOC-.,E-94---SPIP-A'Tio@3 ACTIVATED SLUDGE MOWD UOUOR Date Obtained 3 -,2/ -cl'? Date Used 3 -2-1-ci Mixed Uquor Suspended Solids (MLSS) L4. 014 g/L I ,o@.-I a I zql cllyts MLSS in final test solution g/L Adjusted to InitiaplH I (isttestsoin.prepared) FinalpH Comments g/L (lastsoln.prepared), TEST SUMTARICE Sample Description 300,3 AF FF InitiaplH of highestconc. tested(looovt-,It,- Comments Adjusted to pH REFERENCE SUBSTANCE Sample Description c- C)(-C)i2 v "C> InitiaplH of stock solution 500 mg/L)- Comments Adjusted to pH EXPOSURE CONORMNS Test Duration 3 VlouC,5 Test Temperature Range: c Comments ENVIRONMENTAL LABORATORY OECD ACTIVATED SLUDGE RESPIRATION INHIBITION TEST #209 TEST SOLUTIONS PREPARATION Test Substance: F'c--3oo5 RF-FF Sample Description: C.0- @AQ-VN @or%nc,,@IV% k a Analyst: Dits: --vv_ 5 -d/-97 Test Conc. mg& mg added 22r 500 mL LLM11 r4 5 .t W4 r mL syn. sewage 92r 500 mL feW p2r SM mL mL microbw inoculum per 500 mL ck TotalVolume mL 50 loo 5'00 /C?cc) coo '50 A50 1.500 500 2q ol.?q girg oqrq 9 g,4/ t;lgq ro ekci 2CO '2@ 2m 2zo -zco TOO 5cc) 57co c3co 500 OECD ENVIRONMENTAL LABORATORY ACTIVATED SLUDGE RESPIRATION INHISITICN TEST LR (>3 #209 RAW DATA Test Substance: Fc-30C)a AF4:p- Source of Activated Sludge Mixed Liquor: N\,Apcn cz@cAtes6.@t@@Tri:rfvln-'e--I 15@, f>cx Date Received: cl-7 Date Used -2 1-9--7 m Analyst: 30-MINUTE EXPOSURE Test Substance -- Concentration(r!@IL) 0.5 1.0 DISSOLVED OXYGEN CONCe4TRATIONS, TIME-MINUTES I 1.5 2.0 2.5 3.0 3.5 4.0 mg/L 4.5 5.0 @ Temp 5.5 OC BK CONTROL 1 lo 15C) I0c) sc:@o /OM 1 c>co BK CONTROL 11 -7.3 4.1 4.2-, k.,C@i-.o T,(. 5. 1 1 L4-S if-0 3-S G.5 ,,I_.S q,? I &1,-L ?--A1- !5.!5 4.9 q 3 3.7 -3LV @@.7 ---(0.3(a.0 s.5 Iq.2 Z.3 16 2.;z 5.9 5.11 4.3 3 L44 .2,9 ;?.q q-3 3,16 2.1 2-3- 1.1 0.9 0.5 -,q 1.3, Q1 -I I--i 1.I- 2o.? 21-o 20. 0.(* 3-HOUR EXPOSURE DISSOLVED OXYGEN CONCENTRATIONS, mg/L Test Substance TIME - MINUTES Temp Concentration(i@tt4 0.S 1.0 1-S 2.0 2.S 3.0 3.5 4.0 4.5 5.0 S-5 OC BK CONTROL I BK CONTROL I C> 50 1C)o Goo 7cco /Cr-O 11 7.o n- g-s-R@'L-1 C.-S (a 5'.3 k94.-4 9 -@ X.00- -7.5 -7.1 1 6--7 5-Li q@s, lq.q -2@0.0 g:+ r.5 '7.'g *7-4 G-9 (o-ST, 4 SIZ 5.'1 5,!1 LiCl /C(.S 7 -7.1 4,4 (103 (0.0 5'.(0s .1 LA.-4 .7- 7.0 6-V (a,14 -o 5.0 r I -LA 8*.o '71 eD 5,7 -7.(t -1 5-91 3.9_JL pH of activatedsludge mixed liquor: pH of highestconcentrationtested: Test temperature: Initial'7.9 Initial -1.9 Final Final VIS Li 19 v II 1%.R ^L. L^OvrvA IV" T CALCULANON OF RESULTS bo TistSubstance: FC-3003 AFFF AnalystT:rudy Stietenhoefer OECD ActivateSdludge Respiration Inhibition Test #209 30-Mlnuto Exposure DissolvedOXV en Concentratons,m3/L ma/L 0.5 1 1.0- 1.5 2.0 2.5 3.0 1 3.5 4.0 4.5 5.0 5.5 Tomp-,c R (1) BBmKK#Il'L 706*.56! 7.3 6.7 6.2 10 6.7 6.6 6.0 S.6 50 7.1 6.5 6.1 5.5 100 1 6.8 6.2 6.5 4.9 500 1 6.8 6.0 5.6 4.9 1000 5.8 6.2 4. 3.4 1000 6.8 5.1 4.3 3.6 BK2 5.1 1 4.6 4.2 3.7 % dififncontrol(s4): 5.3 5.8 5.4 4.9 4.2 3.9 5.1 4.5 4.0 3.5 3.1 4.8 4.2 3.7 3.3 2.8 4.3 3.8 3.4 2.9 2.4 4.2 3.7 3.2 2.7 2.2 2.9 2.4 2.0 1.1 0.5 2.9 2.3 1.6 0.9 0.6 3.3 1 2.7 1 24 1.9 1.4 ECSO (95%Cl)u '>ICPOO vl tL 3.2 2.8 21.6 2.5 2.0 21.5 2.2 1.8 21.4 1.8 1.3 21.1 1.7 1.2 20.8 21.0 20.6 1.0 1 0.6 1 21.0 0.991 1.003 1.067 1.055 1.070 1.276 1.328 0.901 3-Hour Exposure Dissolved OXY gen Concentraflonsm, L ma/L 0.5 1.0, 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 L5.@5 Twp,-c R I BKI 9.0 8.7 8.5 8.2 7.8 7.5 7.0 6.6 10 8.4 8.3 8.0 7.5 7.1 6.7 6.1 5.7 50 8.7 8.5 8.1 7.8 7.4 6.9 6.5 6.2 100 8.2 7.9 7.6 7.1 6.7 6.3 6.0 6.6 500 8.4 8.1 7.7 7.4 7.0 6.8 6.4 6.0 1000 8.6 8.4 8.0 7.8 7.5 7.o 6.7 6.4 1000 8.6 8.4 81 .9 7.7 1 7.4 7.0 6.8 BK2 7.9 7.6 7.2+6.8-1 6.3 1 5.9 1 5.5 1 5.1 % diffincontrol(s4-): 2.4 ECSO (96%Cl)=> (1) R- Oxom umake ride(ma 02A.-min) 6.1 5758.470m 5.3 5.4 4.8 4.4 5.7 5.4 4.9 5.1 4.7 4.2 5.7 5.3 5.0 6.2 5.8 5.4 6.5 1 6.1 f 5,.1981 4.6 4.3 (2) Ra- R &*Ned 1024rC- IFI/s.Ex) (3) % Intdbklon[a(RaCm)-RaW(RaCm)jloo (4)% dowentIsnmurob:(IR&Bkl-R&WL%aCm()T1w0o0contrMoumd bewith1i6n%04G&Cohther.) (6)Mom &dwedA.ammou (RaW+RWWV2 a- 1.072 PAcneM-ean&**ledR,omtmb Ok-blanckoritSr.o*f=,pis Tabs-sampltownp x- Tobs-2(rC 19.2 0.789 20.o 0.882 19.5 0.797 19.9 0.814 19.8 0.686 19.7 0.654 19.8 1 0.575 20.3 0.831 LF; ENVIRNOMENTAL LABORATORY OECD ACTIVATED SLUDGE RESPIRATION INHIBITION TEST# 209 TEST SOLUTIONS PFIEPARATION Test Substance: Sample DescriptioAn:LoP,1CIIC-P4C-0 Lt-16C-1,) LOT Analyst: 7y@c@5 Date: cl -7 Sto& Solution Preparation-600 .5 e-c.4A 1.0 '&,S-DCi7 o.tt4." Acz.2.0ar- @d-J,30yit ik44& 11 p vn t t,3kA s nl o, S tobr,@t! I o t-3 W,\o %-k OC?G 15 I<C:,. Tom Conc, ma/L mL added 22r SOO mL U-,ell 3-21-9-r fol-1.40(Il ;@a*fer mL syn. sewage per 300 mL food oar 500-ML COVD-tooc- Q %0 -A I el a7 q 1 (0 )(0 6,ps@- c-onc- -ke-64,eil mL microbial lnoculum Rer 500 mL -2-c.70 TotalVolume mL 5C>C) ENVIRONMENTAL LABORATORY 99 OECD ACTIVATED SLUDGE RESPIRATION INHISITICN 7ES7 #209 RAW DATA Test Substance: 0'%c-inIc)pokke"C) Source of ActivatedSludge Mixed LiquorM:eAtt3)WQ64o--(OaAer Ti-ecime Date Received: 3 -c2 -7 Date Used: Analyst: -@ .(-5 Pick @7 30-MINUTE EXPOSURE DISSOLVED OXYGEN CONCENTRATIONS, VL Test Substance ---I TIME-MINUTES Concentratio(nftlIL)0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 OC BK CONTROL 1 10 -7.(. -7.3 (*.-1 (o lg,i'L17.9 7. (o -7 S -'5"9.4 li-7 4,*Z 3.9 3.Z 12-4 ;ki-L (0-1 co- (*.(3 s.-I-!14 5.0 R I BK CC*N"RM 11 q,(,-q.-)_3,,7 3.-6 7:,T I.q 1.0 0.16 I.o 3-HOUR EXPOSURE C)ISSOLVED OXYGEN CONCENTRATIONS, mg/L Test Substance Concentration BK CONTROL 1 lo TIME - MINUTES Temp 0.5 1.0 1.5 2.0 2.5 3.0 1 3.5 4.0 -4.5-T-5.-0T- 5.5 oc 19.0 7 -7-s -7.6 2- I.? 'Ilr T-15 I.Li jr.o_ 7.'y *?.S 'I-LA -7.7- @2,0. I SK CONTROL 11 -7.9 pH of activatedsludge mixed liquor: pH of highest concentration tested: Test temperature: Initial '7 ctInitial fr-0 Final 9.(o Final ENMRONMENTAL LABORATORY OECD ActivatedSludge foo CALCULANON OF RESULTS RespirationInhibitionTest #209 (4- 0 Test Substance: 3.6-Dirblorophenot r- Analyst:Irudy Stiefenhoefer m Cl- 30-Min to Exposure Dissolved O)XWV n Comentra onn+s m L ma/L 0.5 1.0 1.5 2.0 2.5 3.0 3.6 4.0 4.5 5.0 6.5- TWOR, Ic R (1) w SK1 7.6 7.3 6.7 6.2 5.8 5.4 4.9 4.2 3.9 3.2 2.8 21.6 0.991 10 8.2 7.9 7.6 7.2 6.9 6.7 6.4 6.0 5.7 5.4 5.0 21.0 0.630 SK2 5.1 1 4.6 4.2 3.7 3.3 2.7 _2.4 1.9 1.4 1.0 V-0.6 21.0 1 0.901 % diffin controls(4): 5.3 3-Hour Exposure Dissolved Oxv en0Concentrationsm, L ma/i 0.5 011*.00 1-1*.55 2.0 2.*55 3.,0 cl3u.,5 4r.,100.'.O.l 4.6 5.0 5.5 Tmp, -c R 1 BKI 9.0 8.7 8.5 8.2 7.8 7.5 7.0 6.5 6.1 5.7 5.3 10 9.0 8.9 8.8 8.6 8.4 8.2 8.0 7.8 7.5 7.4 7.2 19.2 0.78f 20.1 0.38 t . BK2 7.9 7.6 7.2 @6:81 6.3 5.9 5.5 5 1 % diffincontrol(s4): 2.4 (1) R- oxygenuptakemie (nig02&-min) (2) Rik-R &**ad to20-C@-IFV*." (3) % k"bnlon- i(RaCm)-R&W(R&Cm)lloO (4) % doonnoo inmtrols: fiRaSki-RoMMACm]100 (Two comrolemust be wfthin15% of each othw.) (6) Mom &dW*d A. contmbm [RaMI+RWW)t2 a- 1.072 Bk- blankcontroSla, sampis x- Tobs-20'C RaCm- nwan ~ad R conlrob Tobs- sampletamp 1 3.9 L 20.3 0.83 Chain of Custody Record @o 3M Environmental Laboratory Form *35176'. PWO 3M FFra,.cN,.kc.y lly::I,3M AAFdddreds-s @6- City.Slate.ZIPCode 07659 3M Pmjed Title '76" - 3M FacilitCyontact 3M Tei"*one Nm*w Sampled t(Pdnt) Item M 2 r3 r 4 5 (,n-6 7 mple Description c e- Oslo Date Time Matrix Number Containers r ofeach IE oZ 3M Project Lead Li Samples Spli -9 10 11 12 13 Item Relipquiipedpy/@ILIIiation Time 0- Date Shipped Via eceiv@d By/Affillati -1-ui Origina-lAccompanyinSgaMP103 LastPage -orignator -F