Document ZBEKQw3nqV9n8dvJBovMKq4aL

A k 2.36 - 0 3 o S ACTIVATED SLUDGE RESPIRATION INHIBITION TEST TEST SUBSTANCE Identity: Mixture containing Perfluorooctanesulfonate; may also be referred to as PFOS, FC-95, or as a component of FC-3072. (1Octanesulfonic acid) (CAS # 2795-39-3). Remarks: The 3M production lot number was not noted. The test sample is FC-3072. Current information indicates it is a mixture of 1.67% test substance, 33.33% diethylene glycol butyl ether, 29.23% water, 20.83% urea, 5% sodium octyl sulfate, 3.33% sulfonated alkyl ether sulfate salts, 4.60% acrylic foamer, 1.67% triethanolamine, and 0.33% tolyl triazole. The following summary applies to the test sample as a mixture of the test substance in water solution with incompletely characterized concentrations of impurities. Data may not accurately relate toxicity of the test sample with that of the fluorochemical component METHOD Method: OECD Guideline 209 GLP: No Year Completed: 1995 Analytical monitoring: Dissolved oxygen, temperature and pH. Statistical methods: Results were determined by calculation of the % inhibition in respiration rate. Test organism source: Activated sludge mixed liquor collected from the Metro Waste Treatment Plant, St. Paul, MN. Test condition: Dilution water: 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 1 N H2SO4 and diluted to 1L with Milli-QTM water. The pH of the reference solution was measured to be 7.0. Test substance was added directly to the test vessels. Test vessels: Not given. Number of concentrations: five plus blank control and 1 reference substance Temperature: 20.7 - 21.7 C Total suspended solids and pH on day of testing: 4.0 g/L (TSS in final: 1.6 g/L), final pH 7.0 Element Basis: Respiration inhibition as determined by oxygen consumption. 002948 Remarks: Uptake rates corrected to 20C for calculations. RESULTS Nominal concentrations: 2 Blank controls, 100, 180, 320, 560, and 1000 mg/L. Reference substance at 10 mg/L. Element values: 30-minute EC50 = >1000 mg/L 3-hour EC50 = >1000 mg/L Element values based on nominal concentrations. Remarks: Testing was conducted on the mixture of the test substance as described in the test substance remarks field. The values reported apply to that mixture and not the fluorochemical proportion-alone. CONCLUSIONS The test substance 3-hour EC50 for activated sludge respiration inhibition was determined to be >1000 mg/L. Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 DATA QUALITY Reliability: Klimisch ranking = 2. This study meets the criteria for quality testing. However, sample purity was not properly characterized and the study lacks analytical confirmation of the amount of fluorochemical proportion in solution. REFERENCES This study was conducted by the 3M Company, Environmental Laboratory, St. Paul, MN, Lab Request number M3597, 1995. OTHER Last changed: 6/25/00 002949 BEST COPY AVAILABLE ENVIRONMENTAL LABORATORY ACTIVATED SLUDGE MIXED UQUOR LR M V ; u / Date Analyst ( ~ /l 2 Page f of ~7 Type Test ^ . r > . 0 Ls, K <k T , ^ A ( i ^ 2 C J \ ACTIVATED SLUDGE MIXED LIQUOR Date Obtained yl?C j c) Date Used 3 / 2 O. f a <T~ Mixed Liquor Suspended Solids (MLSS) H g/L Adjusted to S'L MLSS in final test solution I t 9A. C \ l c} (*\ C .2 .L ) * 2 . - iV\l_` tX-...... I v-i Initial pH m . (1st test soin, prepared) Final pH 7 ( ; (last soin, prepared) Comments ,1 K,, K .t I ^ H .. .\S t-.t o t Jz.______ i. I r r i TEST SUBSTANCE Sample Description F C. ~ ^C- 1 r ) F F f - tv a ( ( --f T - .-.Ikv i- ^ i^ y Cl' I Initial pH of highest cone, tested ( i r r Cujji) = C~- t ' Adjusted to pH Comments ________________________________________________ REFERENCE SUBSTANCE Sample Description R<fg(-v;ioC< Initial pH of stock solution ( I Q mg/L) - 7 , D Comments ________________ " ______________ Adjusted to pH EXPOSURE CONDITIONS 'S ' T e st Duration ~~ FjO r.v>75 Test Temperature Range: OC. 1 - 3 l.~ 7 C Comments S>nl-s t ~ . ' V i c c o i I b ly u 'U A a p n ^ r l ^ .A k s t q-s d i _ Y ~ > i O v 4 k F r ^ a i d i V f o c ' <j a -y p I * \ A d <W.t 4 tatA__ ` Vj r ^ iic k --i i i --3 F p r u ri i'.aiu,** ___ r M ' Ji ft) .tt a I__^ S. \ J ii.`LA.--u^r'i.^1 ;__________ mc. 1~ Ttv L >>Xi____ Iff f y . A l *' ,*-*V,f-T *i > *..J- 'di^i r, *,f-v ' vsr-t-ts>yi * t' V v '- v - ) V vfjv>_ v^*-. *: f fr _ r44*rf $ } - 0 0 2 S S O BEST COPY AVAILABLE 7 ENVIRNOMENTAL LABORATORY OECD ACTIVATED SLUDGE RESPIRATION INHIBITION TEST a 209 TEST SOLUTIONS PREPARATION T e si Substance: ____ F c - 5 Q 7 ? _ _______j \ F F f ____ B < x s ^ ''-3 Test Conc^ -m t added m l MQ(1) water ~%^sawL-^ per 500 mL per 500 mL T ---- mL syn. sewage feed per 500 ml mL microbial inoculum per 500 Total Volume m-L____ i . ^ `-m l p ff V M ' <k . C f i i V C (l O C O .^ lL } -- 1~ , .........^ p M ____ t" A ijo r'/.n i. "fo 7 iq .............................-- -- A.V-J-V1 VtiMi"' - , y/2`X.-r-' i' W * ; :' . ; v , .--FF - v : ' (1) Millipore Millt-Q^ high pui tty water , ^ A Jj BEST COPY AVAILABLE ENVIRONMENTAL LABORATORY 'LR OECD ACTIVATED SLUDGE RESPIRATION INHIBITION TEST #209 RAW DATA A 7r V7 1 Test Substance: ~~~ C . ^ - 0 / 7_ /A t \~ t~ k . t M L . _________________ Source of Activated .Sludge Mixed Liquor: r- 2 - - U- - - '. -- - 1 r - r' Date Received: - / /7 Date Used: 2' Analyst: _____ ( A ________ / 30-MINUTE EXPOSURE Test Substance Concentration (- .j i - ) 0.5 1.0 DISSOLVED OXYGEN CONCENTRATIONS, mgL TIME- MINUT ES 1.5 2 .0 2.5 3.0 3.5 4 .0 4.5 5 .0 Temp 5.5 C EK CONTROL 1 C'; '' (', 7 V _k_L r . /" 7 , 7 1 .r c.r. 0 ,6 0 5? S/ r.7 O 2 A- y / A 7" . 7 t 1! i7>2 7 7 ; w .- Y 7L ^ 7 - '-/ ^ r <2 ' / ! '2_ /. 7 7 7 v /. S~ ? /A . it y EKCONTROL II c . \ *9. 8 - L 7 I 4 . 7 M 7 H .O ? C' 5 . 2 , 2 7 z . Q t A 7 3-HOUR EXPOSURE DISSOLVED OXYGEN CONCENTRATIONS, mgrL Test Substance TIM E - MINU TES Temp Concentration (^j L ) 0 .5 1 . 0 1 . 5 2 .0 2 .5 3 .0 3 .5 4 . 0 4 . 5 5 . 0 5 . 5 C EK CONTROL 1 O .i 6 .0 S ,G M .6 Ll . l 3 .T 3. i 7 .7 lO A 1*0 320 S00 ^ J j L 5 . c J A. G 7 . i 5 ,3 5 . 0 2 . 3 7 , 3 ( * '? 2 f . 2_ S L -5 - 7.Z . VT 5 . 3 ? , o J . 7 2 . 4 2). Z J5_2_ J L 5 L I,0! M , C 7 ,7 7 Z 7, S 7 /, / 1^,3 6 ,1 _ .S ,^ .7 ,7 7 ? Y p H 7 3.<? 5 . s : }0 . 7 `. c & ______ ; iL L 7 , (s 5 - 7 3 , 3 J . 7 2. ^ 1 . ( 7 1 . 1 EK CONTROL II cV l SM L J L A 3 C o 3 .& ; 5 . 1 7 - ^ 2 - 7 7 0 . 7 pH of activated sludge mixed liquor: Initial ~s7~ pH of highest concentration tested: Initial___ - C) Test temperature: J O . 7 Ac .,11.7 XC.fZ**Y!f-*Z' r. a A A A ' 7 2 Final,, ^f^S-Final / . I * ' 11# ' V- 2 & .'iVf'-'-.Vi' V - *7 ' BEST COPY AVAILABLE ENVIRONMENTAL LABORATORY OECD ACTIVATED SLUDGE RESPIRATION INHIBITION TEST #209 CALCULATION OF RESULTS Test Substance: FC-3072 AFFF BASE Analyst: GWJ V VL*t , Lr: M252Z . Date3: k3l/2 0 /9 5 v^v mg/L 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 Temp, "C R (1) Ra (2) % Inh. (3) BK1 5.9 5.5 5.1 4.8 4.5 4.1 3.7 3.4 3.0 2.7 2.4 100.0 6.4 6.1 5.7 5.3 5.0 4.6 4.2 3.8 3.4 3.0 2.6 180.0 5.0 4.7 4.3 4.0 3.5 3.1 2.7 2.4 2.0 1.6 1.2 320.0 1.0 0.6 1 560.0 0 .6 1000 0 .8 BK2 6.1 5.8 5.4 5.1 4.7 4.4 4.0 3.6 3.2 2.9 2 .6 % diff in controls (4): 7.1 EC50 (95% Cl): > \ O C O ^ / L 21.2 20.8 20.7 21.5 21.6 21.7 20.7 0.6958 0.7745 0.7770 * /VA _ /V A ._ a/ A 0.6401 0.7326 0.7401 hIA a/ a M -10 0 0.7212 0.6870 RaCm (5): 0.6635 3-Hour Exposure ______ ______ ______ Dissolved Oxygen Concentrations, mg/L mg/L 0.5 1.0 1.5 2 .0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 BK1 6.2 6 .0 5.6 5.3 4.9 4.6 4.2 3.8 3.5 3.1 2.7 100.0 5.6 5.2 4.9 4.6 4.1 3.8 3.4 3.0 2.7 2.3 1.9 180.0 5.4 5.1 4.8 4.5 4.2 3.9 3.6 3.3 3.0 2.7 2.4 320.0 5.8 5.5 5.2 4.9 4.5 4.2 3.9 3.6 3.2 2.8 2.5 560.0 6.3 6.1 5.8 5.5 5.2 5.0 4.7 4.4 4.1 3.8 3.5 1000 5.3 4.9 4.6 4.3 4.0 3.7 3.3 3.0 ^ 2 . 7 2.4 2.1 Temp. 'C R (1) Ra (2) % Inh. (3) 20.8 21.2 21.2 21.1 20.8 21.1 0.7261 0.7406 0.6000 0.6703 0.5709 0.6303 0.6868 W r - - 0.6813 -"v. 0 0.5520 2 0 v 0.6210 f e 1 0 -- 0.5400 * $ * 2 2 0.5839 15 BK2 6.1 5.7 5.4 5.1 4.6 4.3 4.0 3.6 3.2 2.8 2.5 20.7 0.7248 0.6904 % diff in controls (4): 0J5 EC 50 (95% Cl): | C C O . 3 / L R a C m (5): 0.6886 ( 1) H Oxygen uptake rate (mg 0 2 /l-m m t (2) Mas R adjusted to 20 C- (R'o x] (3) ' Inhibition* ((RaCm)-RaS'(RaCm)JlOO (4) %difference in controls flRaBM-RankPf/RaCmJtOO (Iwo control* musi tm *v/fbm i.*.5- of each other ) (5) Moan adiusied M. con;rols= [HaHk 1RaBk.?}'? o= 1072 RaCms meanadjusfed R. Controls Bk= blank control. S* sampte Tobs* sample tomp i= Tobs-20C * Hh * A/et I 'A c<\l c a l a l i . . ~ Jr>3. BEST COPY AVAILABLE T :;) ENVIRNOMENTAL LABORATORY LR >'M ' i OECD ACTIVATED SLUDGE RESPIRATION INHIBITION TEST #209 TEST SOLUTIONS PREPARATION '1 7 Test Substance: 1 f ^ * C l\io~Q p I Cl T t f t V *v. c e Sample Descriotion: Ccc! L A L'y- 1 A I A 1. a . C /-.--V \<:cl 1 !. L ; T C C I >1_ t/, Analyst: f - Date: // Stock Solution Preoaration: ; iP - Pc' P __ i U L . c +__ : \* ^ Pi !A A ! i O 1V ' U . v -*I* *.*-- *\p r .j .\ 11 P CL ~V_>^C _V l AP_ - 7 c______ :___ 1* t O' 'tf * *'i ' t : L lw = 'i`C0 .A.^/ i-. 1-VVL = C Lj y X V !'* v - P' .7.` f i " * l' - r Test Cone. mL added ma/L oer 500 mL ' C.-.'L !1 ----- lC .. . ILL A = X ---- mL MQ(1>water mL syn. sewage oer 500 mL feed oer 500 mL - v4 *C: ' I i r- : h ______ i i _______ mL microbial inoculum Der 5C0 mL ~:C C ! i Total Volume mL .rr*" ; ! i; _____ W L ______ -- X L 's yjjih s ' _________ 7 -----a ^ fs V -Jr S r ..\^ I L ^ SZziX C'P pH -- 7 .-A - y 7 t*1 rpT -1-- (1) Millipore Miili-Q^ high purity water PPPPPW-T;l Xi\V"l' PPPIITTc.c A l-i A I : : .v*.' . .-v. ^ *v r * s l, V * ./ ; ir I * :s';" w - urite** * s'J Hfit- t V'"*'' *' >, * ; ; o o 2 s s f I I S BEST COPY AVAILABLE 7" t r i 7 ENVIRONMENTAL LABORATORY LR lH ^ S c't 7 OECD ACTIVATED SLUDGE RESPIRATION INHIBITION TEST #209 RAW DATA Test Substance: Source of Activated Sludge Mixed Liquor: Date Received: ' / - i/ I '" Analyst: X 7 r , ' . i.U-,k> U ' i - ^ I < - . f Date Used: - ) ^ 7' L J 30-MINUTE EXPOSURE Test Substance Concentration ) 0.5 1.0 DISSOLVED OXYGEN CONCENTRATIONS, mg/L TIME- MINUT ES 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 Temp 5.5 C BK CONTROL 1 If 1 7T X V m .t X l " 7 7 f- X X L L Z . X 7 7 XX ss L - 7 - i y. ::t 6 ;x L X 7 BK CONTROL II ^ 5 X 7 ,\ X 7 M X >-X : '1 ; .6 x c . ? 3-HOUR EXPOSURE DISSOLVED OXYGEN CONCENTRATIONS. mgL Test Substance TIME MINU TES Concentration (;..y L ) 0.5 1.0 1.5 2.0 2 .5 3 .0 3 .5 4 .0 4.5 5 .0 5 .5 BK CONTROL 1 1 6 . 2 . (? , 7 . 6 S . 3 4 ^ 4 . 6 4 - 2 X J L L . _ 1 _ L 7 .0 6 7 6 ( T t 6 7 I 6 3 3 .T 3 . \ 7 7 c , i S \ c| Temp C x > .% xi 1 BKCONTROL II C . [ > '7 S.q pH of activated sludge mixed liquor: Initial 7 -- n pH of highest concentration tested: n Initial 2 3 2 Test temperature: J t . 1 ----- 1 \ X C . X- q .3 4 . 0 3 .6 >.Z- 0 . 3 -e rr* 7 Final m sx ---2 .7 it BEST COPY AVAILABLE L j*L ENVIRONMENTAL LABORATORY OECD ACTIVATED SLUDGE RESPIRATION INHIBITION TEST #209 CALCULATION OF RESULTS Test Substance: 3.5-DICHLOROPHENOL Analyst: GWJ 30-Mlnute Exposure ______ ______ ______ Dissolved Oxygen Concentrations, mg/L mg/L 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 BK1 5.9 5.5 5.1 4.8 4.5 4.1 3.7 3.4 3.0 2.7 2.4 10 6.6 6.4 6.2 5.9 5.7 5.5 5.2 5.0 4.8 4.6 4.3 l Lr: M3597 Date: 3 /2 0 /L 3 Temp, X R (1) Ra (2) % Inh. (3) 21.2 0.6958 0.6401 21.4 0.4606 0.4179 37 li'i BK2 6.1 5.8 5.4 5.1 4.7 4.4 4.0 3.6 3.2 2.9 2.6 % diff in controls (4): 7.1 3-Hour Exposure ______ ______ ______ Dissolved Oxygen Concentrations, mg/L mg/L 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 BK1 6.2 6.0 5.6 5.3 4.9 4.6 4.2 3.8 3.5 3.1 2.7 10 7.2 7.1 7.0 6.8 6.6 6.6 6.4 6.3 6.1 5.9 5.8 20.7 0.7212 0.6870 RaCm (5): 0.6635 Temp, X R (1) Ra (2) % Inh. (3) 20.8 0.7261 0 .6 8 6 8 21.2 0.2909 0.2676 61 BK2 6.1 5.7 5.4 5.1 4.6 4.3 4.0 3.6 3.2 2.8 2.5 % diff in controls (4): 0.5 20.7 0.7248 0.6904 RaCm (5): 0.6886 (H fU Oxygen uptake rale (mg CV'l-mm) i? i Ra* H adjusted to ?0 C - fR/n f ] (3) % tnhibrttonr |(RaCm)-Raiv(MaCm))100 ' 4) difference in controls R.0k1-RaPk?l/R,if;mll0Q (Two o c tro is rmj-.t l-o wiihm IS". >1 each other ' Moan adjusted R. controls: [RaRkl*RaHk?|/? o " 1 072 : HaCm= mean adjusted R, controls \ Bk* blank control. S sample Tobs-^ sample temp *= Tobs-20C , C*> BEST COPY AVAILABLE IX NaOH T o ta l C o n ta in e rs| of Each Item 4.56Z00 OOA Chain of Custody Record 3M Environmental Laboratory .. ....... T i V r M c v o P Art..:''*. v v.'-v 'V. `V..<>. c u r j1 '' 02663 3MOOQuOStCf jmproicct Lead ! ,j 3MProbet Number ________ 3MDepartmentNumber LabReq^PStTompiatONumber -g-*:.;'-*' fa x ! s , -* , "\teprt ^Sample Description 1 Y fvi 2 3 4 5 v<L ^ natc C7 i , l T ^ \2 J Date Time Matrix / /. iitfa --' n *--------I T!~ Number Containms of each V P re s e rv a tiv e * -, 3 O c o 2 n X0z 8X|S( l/>n 7, j - - - -- --- -- -- i! Z- Sam ples Split See A ttachm ent Comments 6 7 8 9 10 11 12 13 j I i ;j i ! I . .L j 1 1 | 1 1 .! Item # Relinquished By/Affiliation Time .Date A/ -- -----r^ ^ ^ ....... J 7 ...;3 M fc Shipped Via -- k\ Received By/Affiliation / ) fj\)Z Time 1 :? /? Date ... i, j" ' 3 /2 w r II ------------- ------------ -- See Reverse Side For Instructions