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ACTIVATED SLUDGE TEST SU RESPIRATION INHIBITION TEST Identity:Mixturecontainingperfluorooctanesulfonawtheich may alsobe referredtoas PFOS, FC-95, or as a component of FC-203FC. (1Octanesulfoniaccid)(CAS # 2795-39-3). Remarks: The 3M productionlotnumber was not noted.The testsample isFC-203FC. Currentinformationindicatesitisa mixtureof0.85% PFOS, 17% diethyleneglycolbutylether,74.46% water,2.34% acrylifcoamer, 1.7% alkylethersulfate2,.55% sodium octylsulfate0,.12% sodium nitrite0,.09% sodium molybdate,0.85% triethanolaminea,nd 0.04% tolyltriazole. The followingsummaty applies to a mixture with incompletely characterizedconcentrations of impurities.Data may not accurately reflecttoxicityof the fluorochemical component of the testsample. MET @OD Method: OECD Guideline209 Test type: Staticacute GLP: No Year Completed: 1997 Analyticalmonitoring: Dissolvedoxygen concentrationtse,mperature,and pH. Statisticalmethods: Results were determined by calculationof the % inhibitioinnrespiratiornate. Test organism source: Activatedsludgemixed liquorcollectedfrom the Metro Wastewater Treatment Plant,St.Paul,MN. Test condition: Dilutionwater: Carbon-filterewdellwater (3M well#2, St.Paul,MN) Synthetic sewage: per OECD method Reference and testsolutionpreparation:A stocksolutionofthe referencesubstance,3,5-dichlorophenowla,s prepared by dissolving 500 mg in 1OmL 1N NAOH, dilutedto 30mL with MilliporMeilli_QTM water,then broughttothe pointofincipienptrecipitatiwointh 1N H2SO4 and dilutedto1L withMilli_QTM water. The pH ofthe referencesolution was measured tobe 7.7. Test substance was added directltyothe testvessels. Test vessels: Not given. Number of concentrations: fiveplusblankcontrol Temperature: 19.1- 20.30C Total suspended solidsand pH on day of testing:4.53 g/L (TSS in final1:.81g/L),initipaHl 8.0 and finalpH 8.5 Element Basis: Respiratioinnhibitioans determinedby oxygen consumption. Remarks:Valuescorrectetdo20*Cforcalculations. RESULTS Nominal concentrations: Blank control,10,50, 100, 500, and 1000 mg/L. The blankcontroland 1000 mg/L were duplicated. Element values: 30-minuteEC50 = >1000 mg/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 FC-203FC 3-hour EC50 foractivatedsludge respiratioinnhibitiownas determined to be >1000 mg/L. Thisconcentrationinhibiterdespiratiobny -13%. Submitter: 3M Company, EnvironmentalLaboratory,P.O.Box 33331, St. Paul,Minnesota, 55133 DATA QUALITY Reliability:Klimischranking= 2. Thisstudymeets allcriterifaorquality testing.However, sample puritywas not properlycharacterizedand the study lacksanalyticaclonfirmatioonftheamount offluorochemicalproportioninthe solution. REFERENCES Thisstudywas conducted by the 3M Company, EnvironmentalLaboratory, St.Paul,MN, Lab Request number R1335, 1997. OTHER Last changed: 6/26/00 ENVIRONMENTAL LABORATOFly ACTIVATED SLUDGE MIXED UQUOR !L-RR 13-55 Date Z -;tq-9-7 Analyst -% V-s Page I of-%- Type Test -OC-r-O RC-TIVATE@) 5WOGE: 9--E@SPIRATIDIO TOD 141151Ti 0 r,)TC-i T O@@ Ac,nVAMD SLUDGR= MIXED UOUOR Date Obtained3 -;t,4-9-i Date Used Mixed Uquor Suspended Solids(MLSS) 44,S 3 g/L MLSS in finaltestsolution 1.71 g/L InitiaPlH V,C)-(lsttestsoin.prepared) Comments -cl-7 Adjusted to FinalpH g/L (lastsoln.prepared).-'. TESTSUBSTANCF. Sample Description F-c- 2o,3 FcInitiaplH of highestconc. tested low Comments A FFF Adjusted to pH REFERENCE SU13STANCE Sample Description InitiaplH of stock solution 5C@D Comments o iro V"%,e h C) mg/L) '7.-7 Adjustedto pH F-XPOSURE CONDMU Test Duration 360t.,@t%-5 Test Temperature Range: 19.1-0?0.3 c Comments ENVIRONMENTAL LABORATORY LR- R OECD ACTIVATED SLUDGE RESPIRAT;ON INHierri()TNEST #Mg TEST SOLUTIONS PREPARATION Test Substance: Fc- o?oaFc, A Sample Description.:90"eh -qu" Analyst: Date: TowConc. nV added MOIL per 500 mL le-co"Yilzot_ - Wei( gilmto:(4wator mL syn.wwage per500 mL foodgar500 ML qs4, mL microbial lnoculumg2r500 mL TotalVolume ML 0 CAgq tcc@o SC70 RT4 -TKi-A ct0 12W O-C ,@j Son 5co -5c)o EC5>Z) Molitpefe-muQmR high parei, 3-zq-9'7 T4@_5 ENVIRONMENTAL LABORATORY OECD ACTIVATED SLUDGE RESPIRATION INHISITICN TEST #209 RAW DATA Test Substance: -rc-2.0,3 A FF F Source Of Activated Sludge Mixed Liquor:me-A@ro LaDa-5.6-L:)a@er-Irypa rne&taPickKt St.R@tj Date Received:.,3- Rq-9-7 Date Used: 3 -o7t4-9 -7 Analyst:- -T(45 30-MINUTE EXPOSURE DISSOLVED OXYGEN CONCENTRA71ONS, mg/L Test Su nce TIME-MINUT,Es. Temp Concentratio(nI)IL) 0.5 1.0 l.S 2.0_ 2.5 1 3.0 3 5 4.0 4.5 5.0 5.5 OC BK CONTROL I /00 5-0b /000 /000 BK CONTROL 11 -7 -ig 74. '7@Li 7.1 (a- 7., (o-y !@.-3 T.g T. 7. f -7.4 G -j? S.9 1'7.o (D.C. (0.'L CO 'g 5.9 5 i4 'f-V 4.1 3:::;3@o 2-3 1.,4 57.1 q-44 .3.R -1.2- z 4;1 (0-1 5.9 5.L( 6-1 q.,7 f 1 L4.-1414.2- 3.-+l3 iR SLI S.o 14/.(.04. 1 3,1 I.A 5.-3 q -If 1-1 4 -cl I q.S 1 '4 .1 3.-4 3, k -3.3 1.91 2.4 O.G - - - J. Z 1 1,9 .0-1 -1 ."7 1.1 c4 20-2. 2 0. 0 C) C) 3-HOUR EXPOSURE Test Substance Concentration DISSOLVED OXYGEN CONCENTRATIONS, mg/L TIME - MINUTES - -------- -- -- 7- 0-5 1.0 1.5 2.0 2.5 3.0 1 3.5 4.0 4.5 5.0 5.5 BK CONTROL I 10 50 /co 7c>oo BK CONTROL 11 -@G 6 -g. 6-!9 -7.1 -7 -5 -7.9 92, 2-3 .4 '6 1 s-g -5.5 T-1-7.-5 &.9 (o -t@, .-7.-5 (0-9 (.S 4.3 7.cl -7 7.'!)--7t.-) 4, '7.-4e 11 -7 5:3 .2- i4.l6 q.-4 .5 L1.9 3 4.21 !5@4 If.5' 11-o 5.16 .2.ct 07.S 3.9 -.3S r--l -o -6.1 5.o 14.@j L4 pH of activatedsludge mixed liquor: pH of highestconcentrationtested: Test temperature: 19.*3 - @0,12- Initial 'S@.0 Initial Final Final T.s Temp oc 2o.l. a 0,11 ig.-i T:NVIHUNMENTALLABORATORY CALCULATION OF RESULTS OECD ActivateSdludge RespiratioInhibitioTnest#209 TestSubstance: Analyst: Trudy -Stiefenhoefer Q6, 30@-Mi uto Emoosure Dissotved Oxyqen Concentrations,m- L m /L 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 TomE,*c R (1) BKI 7.8 7.6 7.4 7.1 6.8 6.3 5.9 6.4 5.1 4.7 4.2 10 7.1 .6.8 6.3 5.9 5.5 5.1 4.7 4.2 3.7 3.2 2.8 50 7.6 7.4 6.8 6.3 5.9 5.4 5.0 4.6 4.1- 3.7 3.3 100 7.4 7.0 6.6 6.2 5.8 . 5.3 -4.9 4.5 4.1 3.7 3.2 500, 6.8 6.3 6.9 5.4 4.8 --4.4 3.8 3.3 2.9-- 2.4 1.9 10 4.1 3.7 3.0 -2.3 1.7 -1.1 -0.6 lioool s BK2 6 m 3.8 - 3.2 2.2@_ 2.1 1 1.7 1.1 0.5 - % diffin controls(4): 3.9 ECSO (95%Cl)= (c)co"i It- 19.6 20.2 20.0 20.0 19.9 20.2 19. 0.7770 0.8848 0.8958 0.8400 0.9903 1.2457 R 3-Hou rexposure m /1 0.5 1.0 1.5 2.0 BK1 7.6 7.3 6.9 10 6.6 6.2 5.9 so 6.8 6.5__ 6.2 100 7.1 6.7 6.3 500 7.@@- 7-.3---6F-9 1000 E887.,.9 7.6 f 31000 8.92I 7.9 7.6 8.1 7.6 7.4 % diffin controls(4): 1.0 6.5 5.5 5.8 5.9 6.6 -6.9 7.3 7.0 (1) R- Oxygm LWW* rat* (mg 02A-ngn) Dissolved oxvien Concentra 2.5 3.0.1 3.5 -4-.60- I- 4.5 6.1 5.7 5.3 4.9 4.5 5.1 4.7- 4.2 3.7 3.3 -5.4 1 5.0 4.6 4.2 3.8 5.5 5.1 4.7 4.2 3.9 6.3 5.8 5.6 5.1 4.8 6.5 6.3 5.9 5.4 5.1 1 .0 .8 6.3 -6.0 5.7 6.6 6.2 5.8 ..5.4 5.0 ECSO (96%Cl)n ons. mj/L 5.0 5.5 7 4.0 3.6 2.9 2.6 3-4 2.9 3.5 3.1 4.4 4.0 4.7 4.5 5.4 1 5.1 4.6 4.2 T c 20.2 20.2 1 19.9 19.8 19.7 19.3 19.7 -19.6 (2) Ra- R adjwod to 20*C. [pio.Exj (3) % InNbkicn.[(R&Cm).PA&(FI*Cm)lioo (4) % dwerence Inoor*ob: (IRaakl-RaMQVRaCmjloo (Two odrdrole must be wkhin 16% of each other.) (5) A4*m adimted R. conudso (RaBkl+RaBk2y2 0* 1.072 RaCMe mean ad)Mod R, coctrok Men blank ewrot. S. Tobs. sanot tomp sample x- Tobs-20'C R (1) 0.8194 0.8485 0.8000 0.8036 0.7285 0.7127 0.6315 0.7782 R LR ENVIRNOMENTAL LABORATORY OECD ACTIVATED SLUDGE RESPIRATION INHIBITION TEST# 2Cg TEST SOLUTK)NS PREPARATION Test Substance: Sample Description:A@k-rc'cii- r Analyst: V-5 ct6 e Date: -7 Stock Solution Preparation: Scx:@e-,aiL, SC)O 3.5-Cc@p lor, ACIA, u@(UAF-ci.-@o -k.0 Ij @-k-,Pso4 I-C)L- '%.I :@Q '%%MC SAr-@k. se,I q " -- 7.-7 >i-:oq- c@(oI s Test Conc. mgA- mL added p2r 500 mL bLk- C-Ov-@rQc>(- - mL MO(l) water mL syn. sewage p2r 500 mL feed enr 500 mL RT(4 116 mL microbiaj inoculum per 500 mL -10 1(D Q -7L4 ((0 @ek4 keS4 C-C":C)--teff,-7(.;'7e4 TotalVolume mL 5C)o (1) MilliparMeilli-ORhigh puritywater L-R ;:.NVIRONMENTAL LABORATCRY OECD AC71VA7&=-D SLUI)C-E :IESPIRATICN !NHISITICN -E---7-209 RAW DA7A Test Substance: -e-l-Nevi c;o Source of Activated Sludge Mixed Uquor: hap. Date Received: -4- .1,@(:-c?7 Analyst: -TV-5 -@@i-rram-e *Lt P(O Fc Date Used: 3 --2-(-491_ 30-MINUTE EXPOSURE DISSOLVED OXYGEN CONCENTRATIONS, mgL Test Substance Concentration(@ii-) o.s 1.0 1.5 2.0 BK CONTROL I /0 7,Y '7- -7,@5 7 .1 (o -el (o.(o TIME-MINUTES 2.5 3.0 3.5 4.0 4.5 1 @55O.-0TS S..S S.q 16'-l I q.,? Ill. 2- ','r-3 5.1 i4,p (4-5, @Temp oC 1 rt.f. 2 o-3 SK CONTROL it cls.3 19- 41 1 3--l .3.-4 ;2.? 3-HOUR EXPOSURE DISSOLVED OXYGEN CONCENTRATIONS, mgtl TestSubstance Concentration(p SK CONTROL I - Si-SOLS TIME - MINUTES Temp .5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 OC - - 7,(, (o.9 .5.-7 5.3 i'9,o -2-o 'W.y 9.5- a-Li zr.3 9,1 71? 1 '7'7 BK CONTROL 11 (0. -@@(=4 5,0 INO pH of activatedsludge mixed liquor: Initial B.o pH of highest concentration tested: Initial 9 Test temperature: ct,1 --070-'5 Final-gc, Final r-J-4vlm%-"PAIAtlN.UkbUfiATC:)RY CALCULKNON OF RESULTS L+ @est Subs'tanice3:.5-Dichlorgablopi Analyst:Trudy_ Stiefenhoefe OECD ActivatedSludge RespirationInhibitionTest #209 30-Minuto Ex *sure m /L 10.5 1.0 -2.0 BKI 7.8 7.6 7.4 7.1 10 7.3 7.1 6.9 6.6 C)issold Oxy ien Co entrations,m 3/L 2.5 3.0 1-3.6 4.0 4.5 5.0 5.5 T. -c 0 (1) 6.8 6.3 5.9 5.4 5.1 4.7 4.2 @- ig"619@.'6*c 0..77777700 6.2 5.9 5.6 5.3 5.1 4.8-'-4.5 20.3 0.5891 BK2 6=6.66 6.1 % diffin control(s4): 3.9 4.9 4.41 4-0 3- 2.8 1 2.4 20.2 1 0.8421_ 3-Hour E osure .m /L 0. ...1.0- 1.5 -2. Dis olved 0 2.5 3.0 3.5 en Co 4.0 entrationsm,gL 4.6 5.0 _5_.5--i Tamp, IC BKI 10 87..96 7.3 6.9 - 6.5 6.1 5.7 5.3 4.9 4.5 4.0 3.6 20.2 9.0 9.0 8.8- 8.5 8.4 8.3 --B.l 7.9 7.7 1 T6- R 0.8194 0.3333 BK2 a. 1 7.6 7.4 7.0 ti-6 % diffin controls(4): 1.0 1 5.8 (1) Fi- OxYgOn 4*Ww rate (mg 020Ln*,) (2) Ra- R ac*Med lo 204-, ipj*.E4 (3) % InMbklonn (4) % 4memnes (s) Mean adAMed l(RaCm).Ra&(RaCM)II00 in awrob: PRWM-RABI,2m@crnitoo R, OmU*io. Wg&d,RaWY2 (Two mmrols must be wlimn on 1.072 RaCne- nmn aqu$W A, conkok Sk- biar* conim, s- ampos Tab" umple twnp 5.4 5.0 1 4.6 1 4.2 16% ot each other.) x- Tobs-20'C 19.6 0.7782 F 60 Chain of Custody Record 3M EnvironmentalLaboratory Form 35176 -PWO 3M Facility 50 Address @c,ityS,tate,ZipCc /@@. L 3M ProjeelTitle 04278 3M Requester 3m ProleLdeito 7M Fac4ilycontact 3M 3M Telephone Number La Wd (PriM) '4 (P- S4MamSpignS.i,g@n.art.u) em -I"mp-Te Description 2 3 4 5 6 7 Contrwor- Number Containers of each Preservatives DaD4atee TiTe @WMraitxrix 0 on z Zx 3@ El SamplesSpliSt E Com om 0 9 10 12 13 Item RelinquisheoA"ffigolpn Time Da@e, Shippedyia Received By/Affiliation Original-Accompanying Samples Lost Page -Ongnalor See R