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_ 0751+ ACTIVATED SLUDGE RESPIRATION INHIBITION TEST TEST SUBSTANCE_______________________________________________ Identity: A mixture containing perfluorooctanesulfonate, which may also be referred to as PFOS, FC-95, or as a component of FC-203CE. (1Octanesulfonic acid) (CAS # 2795-39-3). Rem arks: The 3M production lot number was 519. The test sample is FC203CE (2/21/89). Current information indicates it is a mixture of 1.84% PFOS, 30% diethylene glycol butyl ether, 60.23% water, 2.56% Sultone foamer, 3.1% sodium octyl sulfate, 2.1% polyoxyethylene monooctylphenyl ether, 0.12% sodium lauryl sulfate, and 0.05% tolyltriazole. The following summary applies to a mixture with incompletely characterized concentrations o f impurities. Data may not accurately reflect the toxicity o f the fluomchemical component o f the test sample. M E T H O D _________________________________________________________ Method: OECD 209 GLP: No Y ear Com pleted: 1990 A nalytical m onitoring: Dissolved oxygen concentrations, pH and temperature. S tatistical m ethods: Results were determined by calculation of the % inhibition in respiration rate. T est organism source: Activated sludge mixed liquor collected from the Metro W aste Treatment Plant, St. Paul, MN T est condition: Dilution w ater: Millipore Milli-QTM water Synthetic sewage: per OECD method Reference and test solution preparation: A stock solution of the reference substance, 3,5-dichlorophenol, was prepared by dissolving 500 mg in 10mL 1N NaOH, diluted to 30mL with Millipore Milli-QTM water, then brought to the point of incipient precipitation with 1N H2S 0 4 and diluted to 1L with Milli-QTM water. The pH of the reference solution was measured to be 7.4. Test substance was added directly to test vessels and was apparently miscible with water. Test vessels: Not given Num ber o f concentrations: three plus 1 reference substance and 2 blank controls Tem perature: 2 0 -2 2 C Total suspended solids and pH on day o f testing: 5.033 g/L and initial pH 6.6 and final pH 6.9. Initial TSS of 1000 mg/L concentration was 2.020 g/L, pH 6.6 and final TSS of 1000 mg/L concentration was 2.200 g/L, pH 6.8. 00112Z Elem ent Basis: Respiration inhibition as determined by oxygen consumption. Rem arks: Values corrected to 20 C for calculations. RESULTS________________________________________________________ Nom inal concentrations: 2 Blank controls, reference substance, 320, 560 and 1000 mg/L Elem ent values: 30-minute EC50 = >1000 mg/L 3-hour EC50 = >1000 mg/L Element values based on nominal concentrations. Rem arks: Testing was conducted on a mixture as described in the Test Substance Remarks field. The values reported apply to that mixture and not the fluorochemical proportion alone. C O N C L U S IO N S ___________________________________________________ The test substance 3-hour EC50 for activated sludge respiration inhibition was determined to be >1000 mg/L. Subm itter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 DATA QUALITY________________________________________ __________ R eliability: Klimisch ranking 2. Testing meets all criteria for quality testing. However, sample purity was not properly characterized and the study lacks analytical confirmation of the amount of fluorochemical proportion in the solution. R E F E R E N C E S ____________________________________________________ This study was conducted by the 3M Company, Environmental Laboratory, St Paul, MN, Lab Request number H 14 8 0 -1 ,1990. O T H E R __________________________________________________________ Last changed: 6/26/00 0011Z3 Type Test ENVIRONMENTAL LABORATORY ACTIVATED SLUDGE MIXED LIQUOR L'l'__n i t.wvj__l Date /q n Analvst L ^ ? ^ - lnHtbt4-jrvi Tgafc. Source Mft b f a \*Ia<^"Treakin t r tiir ^ - a y lir ^ ^rV .hAv\. Date Obtained 7^ j \ Q jc \C )___________ Date Used ^ j \Q jC \r\ Mixed Liquor Suspended Solids (MLSS) g/L Adjustment g/L pH Lq-Loj -P.v^al to.Q ._ -- Comments_____________ ._______________________ ^ ' _______________ _ Test Substance Sample Description 1 ^ 5 1 3 //l/gft)----- ;------------ -- VUqHest- cvjZcE?SBovCtj^d SamPle k.ft____ Adjustment-------- -------------- - Comments M l < & n t TOOQnnc^L.4 ac.4i -"SrJiri-^ ..Q^glU Reference Substance Sample Description^ - .T>ic>ilomphgr^i______ UiqWcsjt QMciej^QM.-beQfbdb, IC>fM/L Sampie pH jntt aj w a ! 1z>,2 Adjustment Comnents.Sffnr Wj .- p U M .4_____________ Exposure Conditions Test Duration ^ ^rnnr.5, Test Temperature 2 ( \ - 2 ? , C Commen18____________________________________ u trr t 2 4 o/rn 10020 0 PWO Sample Description Environmental Lab -- Work Sheet OECD ACTIVATED SLUDGE RESPIRATION INHIBITION TEST #209 Lab Request No. iA \M.&Q.~ 1 Page _ 1__ of 5 Date: _ s/ i q / g p Analyst: -----------------------Test Solutirms Prparation---------------------- PC. f (zlu /fft). T<ssfc, rsubstaviff. rJrar yltoudj -rav-ruj --Urlici ) m ifg ibte. v^ith w ater.________________________________________________ :----------- Individual w effite uard......................................................................................................-- ............ X rest Cone, mg added mlMQ water ml syn. sewage ml microbial Total volume mo/L rer 500 ml rer Slffl m l ---- f ^ H npr SIM ml 1nnn.1i. n*r TOfl ..I ZIO lier 4- 2_RLj. w He +- io n = 500 5b 0 ZPO +- *- Ilo -V- 200 - 500 lnoo* 5cc\ P 2ft4 + ile + zoo = 500 BtatOaftfarplI ___a __ +- .- g M \L> t o o _____ " ^500 S n a r e d r ^ f W f c y r A 3T w \ V n L-R, U lM -ftD-5. .. V frij -fo arn tj. b a r y , A rritw tk rrf -Poam -Formgri,---------------------- _ TkLs riu ^ U rrtfM . LL<v*r\ -fo r ~TSS, 001125 ENVIRONMENTAL LABORATORY OECD ACTIVATED SLUDGE RESPIRATION IN H IB IT IO N TEST RAW DATA #209 lr A M 8 0 - J Test Substance: L o t 5 / 9 ( z / z j / Q ^ ) ________________________________________________ S o u rce o f A c t iv a t e d S lu d g e M ix e d L i q u o r : A ^ ^ g W(ksh~ D a te R e c e iv e d :, ^ / / f / f / 7 ___________ D ate U sed: c ^ / / <?/<?/0___________ A na lyst 5 4 p f/? f//-e i^ c 6 /W rtiL < 30 - MINUTE EXPOSURE le s t substance DISSOLVED OXYGEN CONCENTRATIONS maVL - r m z MINUTE s C o n c e n tra tio n (m g/LJ 0 .5 1 .0 1 .5 2 .0 2 .5 3 .0 3 .9 ^ 4 .0 4 .5 5 .0 L,5*5-- ? CONTROL I 7S2n /ft, 4 4 f t 4 , 4 4,0 H.fo 4 , 1 ^ , 7 Z ,R 4 ,9 4 n 2 ft /,S T / , 5 a t w % z,i Zl 1n o n A 5 S ,.4 f,to / 10 / a 5 x . n (.9 0 ,7 zn ZL - CONTROL I I & 2- 4 -f iL 2 u 2 u 2 * L z fy J L J J l . IL 3 - HOUR EXPOSURE DISSOLVED OXYGEN CONCENTRATIONS m o/L le s t substance T I me- mINUTES TEh C o n c e n tra tio n (m g /L ) 0 .5 1 .0 1 .5 2 .0 2 .5 3 .0 3 .5 4 .0 4 .5 5 .0 r5 .5 C CONTROL I X lo O lo r n 5 f t 4 , ( p 5 t h V ? ? 4 S 4 , 1 , * j , 7 4>.Zj z ,4 Z,0 h i (e,\ 5 , 7 5 , * t 4 . 9 4 ( P 4 / 4 , 4 *> 0 Z .(a ? u h PC 4 f t 5 , 4 5 , ft 4 (* 4 ,? ., *>;% 5 , 4 ?u7 P .,4 i f t 2C (p,l 4 (p 4 , Pi 4 f t 4 , 5 4 ? , 4 ,0 2,fa ? X Z f CONTROL I I 5 ft S 3 . 5 ,1 H ite. L L 2 . pH o f A c t iv a t e d S lu d g e M ix e d L iq u o r : pH o f h ig h e s t c o n c e n t r a t io n t e s t e d : T e s t T e m p e ra tu re : ZO -iilLPC In itia l I n i t i a l le><U> 1 ,iq F in a l b . ^ F in a l lp.il f/ jlu . . 001126 ENVIRONMENTAL LABORATORY ACTIVATED SLUDGE RESPIRATION INHIBITION TEST #209 CALCULATION OF RESULTS Test Slihgtanrp & C - CF. jc rt .S /9 fz /z .//% 9)__________ 30 - MINUTE EXPOSURE Test Substance Concentration (mg/L) *>20 .*ln 1000 Oxygen Uptake Rate R i.nisa* I.SIMS l.ltoll R Corrected to 20*C A.5UI/0 I.5K3 \.?>nS l.lum LR / / / v f n - / Date . __ Analyst 1 Inhibition in Respiration Rate^ ---- " 3.S - -T -MS .... vr.. QDBm.il___________ Q/225Q_______ Percent Difference in Controls^ ECjo (95% Confidence Limits) mg/i. ? >rfn o n n b i__ !__ Test Substance Concentration (mg/L) CONTROL I *2 0 .^l^n in n n Oxygen Uptake Rate R 0, r \.T l* A n.m crt o .-m A i R Corrected^ to 2(f C o .n tn is .T 1 *-* o .n o p o .n U Q i 1 Inhibition in ,-) Respiration Rate^J 0 .4 n il ** CONTROL II___________ _____ O ' ^ b O l o ________ Percent Difference in Controls^ ECgj^95%Confidence Limits) mg/L. (1) Temp. Corrections.- ^T.obs (mg 02/L-min.) n rrtt?, (3) % Difference- X 10 (2) \ Inhibition** / - p * X 100 Where: R Oxygen uptake rate (mg 0-/L-min.) T,obs Sample temp.,*C L - 1.047, x - T,obs - 20*C C Control The two control respiration^rates should be within 151 of each other 001127 Solids [TSniSSJfTDSl 3M Environmental Laboratory - Raw Data Sheet (ITttiedi M S to t-T T , Sec. lethod Reference: Std. Methods (14thed.)p 80 08, see. 308 alculation: mg/l Residue = mg residue x 1000 ml sample M'TCed Uc^uor' <1-used. - S r U F $ W l4 8 0 -lJ`5 jli> a- 3,S -J>c# Sample Description + e>Av-doe MetroW *fe rioe&fw^rvd-TW 1 31-.T s u i, M n. 'L Reported Result mg/l ml Sample S Gross Weight after 10'S *C 1. 1 4 3 5 i.\4 n s +W Uer" ffn iflb lt Weight (q) Residue Weight (g) i.u a s 1.1155 0 .0 2 5 2 0 .0 2 5 2 -Hel AFC05CE X l2 3 a f c . w * \.l4 o 4 1. 1 L5 3 o.oz5 i 1. 1 2 M 1 .1 1 3 2 ft.ftift2 s 5 1. i 3 o ft 1.1201 ft. 0101 le m: ;a.PC^09<> OSI? fU*q/L *1 St Solfci<>l\ _____________a 1. 1* 0 ^ 1 1 .1 2 4 1 O.Olftft U Z .^ S 1. 1151/3 0 .0 0 4 4 .*S l. 1 2 5 0 l .t l 2 fi ft , O 1 0 2 j -____________ 3 . 4r In PCiOSCE as0fcG. kUT/flli.rtv./n lr> 5 U 2 2 11 l.lll/sfc O .o i o s 5 1. I S S I 1. 1 2 -41 0 .0 n o ____________LL iX3rvu>H_^'Z*4OiVSHCE A t 60lux*tA. 1~5 ___________ L 5 1. 1 2 5 1 1.1143 ft. ft 104 A 1. l l R I o I.tfti5 ft. ft u 1 -s I . 12S.5 I.U 4 5 n . f t 11 f t 5 i: i2 ? .*\ 1.1114 n . O \1 l ------------------- is . A - 1.1250 1. 1145? f t . ft il 1 Residue mg/l Comments 3 0 4 ft 50 40 5 0 20 2o 4C 2020 000 14 o 2 0 4 ft 2 0 1 /3 0 2200 1 .I S O 2220 2200 2 222) 22 20 V X = 5 0 3 5 : I 2 m ^ /L -3 , 1 ^ "X = D Z D - 2 0 w ^/\o 0 ^ - X = 20Z .T 4 2 ^ L D - 2200--Z O k ^ U 'I v _ _ -------------------------=*----- -->X \Z.rrpL, - arm 10630 8 O -PW O Lab Request No. H W ^ O iample Description S,5-l)ichlo^}jpharto' %W>o fem iC C - ^substawcc. Udr cVt 'T^d. Label MnwatOsee, W > L o t `fc't, 01*0-0 Environmental Lab -- Work Sheet OECD ACTIVATED SLUDGE RESPIRATION INHIBITION TEST #209 Page _ Date: _ Analyst: Stock and Test Solutions Preparation -.3 ) .S-CI^chlorofthcrtpl ^efrrcvtcfi ^ufrsfcfiYlfc&r!t5y-fcHdjSQ STOCK SOLUTION: \wmLi - O .S m j ---------- ____________-riiI.ssK/M .Sfifirij SjS-JDC'fi >n lmLi I.NS NfaDU----- ____________zJiUufceA ii SQim b vjVBi -------------------- ___________ --p A d p iL I.qK UgSCi^ (Wrtpwy.. vsih\ aBnryi^t -- _______ !______ iAcIp f u t p^rlprtftBrq.________________________ :----- ______________ "~ \^j'* A 4 r> Chy\*>. 1i t e r vMrfch M j 1li"Q w a t e r : ----------- S faD C ^ ^ \u t O r t rest Cone. ml stock soin mlMQ water ml syn. sewage ml microbial Total volume rnc/L per 500 ml___ per S00 ml feed per 500 ml inoculum per 500 ml ml _ 1D__________ TQ O -L 14 + -b Z.&H- -V- U*________ _____ L__________" JQ \U>______ ___ 1 . ; _____ - 5Q S h a r e d v S k , C /avtbnrd v o t4 V \ t4 \4fiP > -lg , 001129 ENVIRONMENTAL LABORATORY OECD ACTIVATED SLUDGE RESPIRATION INHIBITION TEST RAW DATA #209 LR .W t f XQ ,, Test S u b s t a n c e : ^ u b Source o f A c tiv a te d Sludge Mixed L Iq u o r: Date R eceived:... *> /iq/< jC )________ A n a l y s t ~ZpihiW r^u_ s f c a ^ C e . ' ) _____ __________________ _ V (asI-f. 'V rf'M m rn ^ .'V \tw L ) Date Used: 5 > / iq ^ p > _________ 30 - MINUTE EXPOSURE fest substance TTmT MINUTE TEMP C oncentration (mg/L) 0 .5 1 .0 1 .5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5-- *C CONTROL Aft AA 4 ft 4,4 4,1 Air? A Z, ft,ft .0 l.lfl u__ in lo .ft b,7i lf?,0 A ft 4,2, S. 4 4 ,2il_ 1 i CONTROL m k-0 .5Ja. j La. L i. ^0 Alo A l A l -LE_ l \ 3 - HOUR EXPOSURE le s t Substance C oncentration (mg/L) CONTROL I I in DISSOLVED OXYGEN CONCENTRATIONS mo/L TIME-MINUTES TEMPI 0.5 1 .0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 .5 .5 C S .ft * V ^ ." 5.1 4.Io 4 ,?( A .ft A A 2 j.ft Zi5 f t . ) l. lo *1 2. 1 1 lo.Q lr?,1 ioXo u 4 (o. A loA 9 4 , 1 , 4 , 4 2,2? CONTROL m ^ 5 _ a o 4 . io 4 i l 2 k la .. J S tL . pH o f A c tiv a te d Sludge Mixed L iq u o r: pH o f h ig h e s t c o n c e n tra tio n te s te d : Test Temperature: 2 .1 - ?9 C . I n i t i a l Ip -Ip I n i t i a l fe.T - L - 1.4 Final (o.c1 Final Ip.8 J A - Uu 001130 ACTIVATED SLUDGE RESPIRATION INHIBITION TEST #209 CALCULATION OP RESULTS Test Substance ) 30 - MINUTE EXPOSURE Test Substance Concentration (me/L) mcRrT V S H H I H H I H - IO Oxygen Uptake Rate R ft. 9 2 ^ 0 _ ft.'SXKZs R Corrected^ to 20 C . ft.H PU Date z jt f f t a Analyst' f*9 * ^ o 7 E 1 Inhibition in . Respiration Rate'-^-' QNrn.ni__________ Percent Difference in Controls^ EC50 (951 Confidence Limits) mg/i- .(a/n Test Substance Concentration (mg/L) CONTROL H Oxygen Uptake Rate R .*> *4 4 2 , R Corrected to 20*C 0^9& Z j 0.31*41 % Inhibition in Respiration Rate'-^' lo \ " CONTROL ITT Percent Difference in Controls^ EC^ (951 Confidence Limits) mg/L. i (1) Temp. Corrections-- --*^' (mg 02/L-min.) (3) % Difference --- f-X 100 f a l * RC^ K i^ !j (2) I Inhibition** / ..... L ^ iL x loo K Re Where: R Oxygen uptake rate (mg 02/L-min.) T,obs * Sample temp.,*C * - 1.047, x - T,obs - 20*C C Control The two control respiration rates should be within 15*1 of each other BEST COPY AVAILABLE 001131
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