Document EqkQkvOe8eXVX9oyRj4oemNyx
O Z 8 H 4 R A A 6 -
ACTIVATED SLUDGE RESPIRATION INHIBITION TEST
TEST SUBSTANCE____________________________________________
Identity: Mixture containing perfluorooctanesulfonate which may also be referred to as PFOS, FC-95, or as a component of FC-3003. (1Octanesulfonic acid) (CAS # 2795-39-3).
Remarks: The 3M production lot number was not given. The test sample is FC-3003. Current information indicates it is a mixture of 1% PFOS, 15% diethylene glycol butyl ether, 79.39% water, 2% Sultone foamer, 1.5% sodium octyl sulfate, 1% sodium decyl sulfate, 0.06% sodium lauryl sulfate, and 0.05% benzotriazole.
The follow ing summary applies to a mixture with incom pletely characterized concentrations o f impurities. Data may no t accurately reflect toxicity o f the fluorochemical component o f the test sample.
METHOD____________________________________________________
Method: OECD Guideline 209 GLP: No Year Completed: 1997 Analytical monitoring: Dissolved oxygen concentrations, 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 Wastewater Treatment Plant, St. Paul, MN. Test condition:
Dilution water: Carbon-filtered well water (3M.well #2, St. Paul, MN) 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 H2SO4 and diluted to 1L with Milli-QTM water. The pH of the reference solution was measured to be 6.3. Test substance was added directly to the test vessels. Test vessels: Not given. Number o f concentrations: five plus blank control Temperature: 19.2-21.6C Total suspended solids and pH on day of testing: 4.04 g/L (TSS in final 1.61 g/L), initial pH 7.9 and final pH 8.6 Element Basis: Respiration inhibition as determined by oxygen consumption. Remarks: Values corrected to 20C for calculations.
002702
RESULTS Nominal concentrations: Blank control, 10, 50,100, 500, and 1000 mg/L. The blank control and 1000 mg/L were duplicated 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 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 EC5ofor activated sludge respiration inhibition was determined to be >1000 mg/L. This concentration inhibited respiration by -24%. Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 DATA QUALITY_______________________________________________ Reliability: Klimisch ranking = 2. The study meets all 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 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 R1331,1997. QUdEB_____ ________________________________________________ Last changed: 6/26/00
002703
ENVIRONMENTAL LABORATORY
ACTIVATED SLUDGE MIXED UQUOR
LR f t 1 3 3 1 Date 3 - a I -9 ~T Analyst "TV-C3 Page J__ of 8
Type Test Q C Q f t C T U / f t lg D 'SLuO G E. & 5 s P t fc A T jo fO "XnOMt 6 lT fC 0 T G S T ^ 2 j
ACTIVATED SLUDGE MIXED UQUOR
Date Obtained 3
97
Date Used 3 - 2 . / - 9 ^
Mixed Liquor Suspended Solids (MLSS1 M. DM g/L
| ,(c| 31 z.qt p r'ts
MLSS in final test solution
^ g/L
Adjusted to _
. g/L
j;
Initial pH 7 *? (1st test soln. prepared)
Final pH * 0 (last soln. prepared) .
Comments ______________________________________________ _
TEST SUBSTANCE
Sample Description
3 0 0 3 A F F F ___________________________________
Initial pH of highest cone, tested (lo o o t ^ li )
Adjusted to pH
Comments ________________________________ _______________________________
REFERENCESUBSTANCE Sample Description 3 X^
1O ^ o p K ^ t o p ^ ______________________
Initial pH of stock solution ( 5 Q Q mg/L) = 0 ,3
Adjusted to pH
Comments ____________________________________________
EXPOSURECONOmOtS
Test Duration 3
_______________________________ _ _ _ _ _ _ _ _
Test Temperature Range: t ^ /3> - 3 . 1
C
Comments _________________________________________ ______ ______________ _
002704
ENVIRONMENTAL LABORATORY
LH ^ ' 3 3 1
P i 2- o PS'
OECD ACTIVATED SLUDGE RESPIRATION INHIBITION TEST #209 TEST SOLUTIONS PREPARATION
Test Substance: P C - 3 0 0 5 f t P P F ___________________________
Sample Description: ^oU*.v> W n , j w
______________________
Analyst:
Date: 3 ' 2 * ^ 1
Test Cone. mg added mart- . w r SQfl mL
Coell.
3-2W-R7 Tiej
m l MQW water mL syn. sewage
pgrSQQmL feed, pec 500 mL
mL microbial
Inoculum Mf.SQfl.mL
e t-<cCOVOTBOL
--
SIZ*J
f(a
'2JDQ
Total Volume ____ mL_ .
ig O O
to
6o
to o 5oo
s
as
5 aso
a i M _____ _ _ t ( a .1 - ..-ap? ______-- _ S p P
l(o '2 0 0
Sop
z m - - J - f a - . . - 1 -1 -3 C O . ------------- _5CO__
aw n,
2jx> _____
5~cp.
tpOO
500
i(n ~ZjOO
5CO ~
500 <3^
. 7.6?.__________acg> ............. -- g 2 Q
f,H ,-r f.
-footed ~ I f r .
(1) Milllpere MllliO^ high purity witar 3 2M-<\n r<es
002705
B E S T C O P Y A V A IL A B L E
ENVIRONMENTAL LABORATORY
LR P3 3
OECD ACTIVATED SLUDGE RESPIRATION INHIBITION TEST #209
RAW DATA
<sr
Test Substance: f - C /- 3 CQ2> A(~FF~_________________________________________ `
Source of Activated Sludge Mixed Liauor: A i\pA<n LOas-W,
Oate Received: 3 -<* / - 9 7
Date Used: ~5
I ~7 1
r Iq ^
7^ - VQ fv \
Analyst:
"T *5___________
30-MINUTE EXPOSURE
Test Substance Concentration (itv^ I l) 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 oc
BKCONTROL 1
lo SO
lo o SCO lo co
IO O O BKCONTROL II
7<p 7 .3 o . l 6.-T 5 7 S-H 4 1 4 x 3 3 3 .TL a *? V I . u
' T f'? 6.0 5.fc S.1 H s <f.o 3 * 5 3 .1
3 O 2 l S
7.1 >5 ( t -I
H Z H i- 4 .7 3 3 X ?
I.E 3 /M
(0 ts 5 . 5 M M H Z 3-M 2.-7 J L _L2_J A 3 , - l i -
(ff'O 5 ,5 4 1
VS 5 .'Z 4 . 3 3 M
H a 3 . 1 5 . x 4 -7 V-2, 1-7 ~L. O M 0 4 --
/.TL 2 0 ? -- ' a /.o
5 ? .MrI 4 3 3 4 <kA
/fe 0 3 o . -- --
2 0 .G
s \ V c , 4 2 3 7 3A> a * 2 -H M l*M /O 0 4 2 / , o
3-HOUR EXPOSURE
DISSOLVED OXYGEN CONCENTRATIONS, mg/L
__
Test Substance
TIME - MINL TES
1 Temp
Concentration (rv^\ u) 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4 . 0 4.5 5.0 5 .5 7 C
BKCONTROL 1
lo O lo o 6 OO /O O O / C O
BKCONTROL II
ro r r
SH * 3 ST?,7L 7 .7
Tt
?. ?.o
?.t
74
7.1 y.o
7 .5
7**
7.1
1^ 7-Y 77
77 7.f
7-H 4T7 .0 l-S 77
/.S' fr,7
<o?>
7.0
7.-H
7 .0
<b-5* 6.
6* T.o
(,-5 6.7
60 GM
M
SM
5.7
SA_ S> 6 .X
6 -S-
S7-
5.4
4.7
S? 6 .|
53 V
20-0
m m ; /7.S M X I9.R 5 .0 14.* S.M" ` ?7 S.S
j -0 I1
'1
>4 ..
7 .Z -
6#
(,3
s .5 s .\ *#4 M 3 M 2 0 .3
pH of activated sludge mixed liquor: pH of highest concentration tested: Test temperature: l*?. X - X I- G
Initial 7 7 ______ Initial 7-*^______
Final Final
______ _____
I j
0 0 2 jb o 6
002707
3s0a :j> h a
u n ii iuiw ici Ira. knDvnniun r
CALCULATION OF RESULTS
4 {..: ~-T' ' ' "
,
Test Substance: FC-3003 AFFF
Analyst: Trudv Stiefenhoefer
OECD Activated Sludge Respiration Inhibition Test #209
lt: h u j I Date: 3 /2 1 /9 7
30Mlnuta Ex
Dissolved Oxy<jen Concentrtons, m3/L
Ima/L I 0.5 1.0 1.5 2.0 I 2.5 3.0 3.5 4.0 4.5 5.0 5.5 Tamp. *C R (1) RaJ2) % Inh. (3)
' X > ,*' %' . \ --'v&Aft'v.'4'V'.Vft,
B I i B i i S S I W
11 l i i l l l i i I M i f c l I I 1 .
BK1 7.6 7.3 6.7 6.2 5.8 5.4 4.9 4.2 3.9 3.2 2.8 21.6 0.9915 0.8871
10 6.7 6.5 6.0 5.6 5.1 4.5 4.0 3.5 3.1 2.5 2.0 21.5 1.0036 0.9042 O --
50 7.1 6.5 6.1 5.5 4.8 4.2 3.7 3.3 2.8 2.2 1.8 21.4 1.0679 0.9688 O
100 6.8 6.2 5.5 4.9 4.3 3.8 3.4 2.9 2.4 1.8 1.3 21.1
1.0558 0.9780 -->____
500 6.8 6.0 5.5 4.9 4.2 3.7 3.2 2.7 2.2 1.7 1.2 20.8 1.0703 1.0124
O
1000 5.8 5.2 4.3 3.4 2.9' 2.4 2.0 1.1 0.5
21.0 1.2762 1.1905
O
1000 5.8 5.1 4.3 3.6 2.9 2.3 1.6 0.9 0.5
20.6 1.3286 1.2743
BK2 5.1 4.6 4.2 3.7 3.3 2.7 2.4 1.9 1.4 1.0 0.6 21.0 0.9018 0.8412
% diff in controls (4): 5.3
EC50 (9 5 % C I)*> i oov^ \ l
RaCm (5): 0.8642
3Hour Exposure
,W S M
m nm
si!m
'> ' V V
< y
BK1 9.0 8.7 8.5 8.2
10 8.4 8.3 8.0 7.5
50 8.7 8.5 8.1 7.8
100 8.2 7.9 7.6 7.1
500 8.4 8.1 7.7 7.4
1000 8.6 8.4 8.0 7.8
1000 8.6 8.4 8.1 7.9
BK2 7.9 7.6 7.2 6.8
% diff in controls (4): 2.4
Dissolved Oxyiaen Concentratiions, ma/L 3.0 1 3.5 4.0 4.5 5.0 5.5 |
7.8 7.5 7.0 6.5 6.1 7.1 6.7 6.1 5.7 5.4 7.4 6.9 6.5 6.2 5.7 6.7 6.3 6.0 5.6 5.1 7.0 6.8 6.4 6.0 5.7 7.5 7.0 6.7 6.4 6.2 7.7 7.4 7.0 6.8 6.5 6.3 5.9 5.5 5.1 4.6
EC50 (95%CI)- > |ooovy u
5.7 4.8 5.4 4.7 . 5.3 5.8 6.1 4.3
5.3 4.4 4.9 4.2 5.0 5.4 5.8 3.9
(1) R Oxygen uptake rata (mg 02/L-mki)
(2) R a -R adjusted to 20*C- [R/a.Ex]
(3) % inhibition i(RaCm)-RaS/(RaCm))100
(4) % dMetence in oontroto: [IRaBk1-RaBk2l/RaCm]100 (Two controls must ba wHNn 1S% ot aacti other.)
(6) Mean adjuatad R, controls (RaBk1+RaBk2y2
a 1.072
Ska blank control, S aampla
x* Tobs-20*C
RaCm maan adjuatad R. controls
Tobe sample tamp
A il 19.2 20.0 19.5 19.9 19.8 19.7 19.8 20.3
|Ra ( E ffflB S l
h illllllilllllli
0.7891 0.8342 !
0.8824 0.8824 0.7976 0.8258
O _____
0.8145 0.8202 0.5
0.6861 0.6957 15.6
0.6545 0.6683 18.9
0.5758 0.5838 29.2
0.8315 0.8144
RaCm (5): 0.8243
ENVIRNOMENTAL LABORATORY
LR R i 53 j
OECD ACTIVATED SLUDGE RESPIRATION INHIBITION TEST 9 209 TEST SOLUTIONS PREPARATION
Test Substance: 3 ~ O
\ o r o p lo e .v A Q 1________________________________
Sample Description: A L Q R i C M C ft(S Q
-OT ^ O Q (o I 5 fc* D
Analyst:
_________
Date: 3 ' 3 ^~ g?~7
Stock Solution
Preparation: S o o ^ g VL. .
l-O ^ I-Q S
0 't> s o K ^ x l S d riirw . B >S-O oP -.n IQ
------------------------------------------------------ -----------------1,0 _frl.sPU____________________i.______
CMu^eA -Vo <xp6ro^^
u? yAU 1W\U - Q
-------------------------------------------- 2 -----
M A f t .Q v n \ 1 1 - 0 t o V W S O d -Vo cla p i r
------------------------------------------- -------------
pv..*uA?.^> l ' o t i
, ' - , ------------------------------------* -
,Fjavtxkf. ^W .3\nrkr *?nl T tp-3 -,
-- ---------------------------------------------------------------------------------
Test Cone. mart-
mL added oer SOQ mL
coeU ,, .f - r i? 7 m t MQv.li water mL syn. sewage
per 500 mL fmj pgr SflO.mL
mL microbial
Total Volume
iPQCUlumD9T5QQmL ----mi__ _
covD iaoc______________ __________________ |_fe_______________ ^ Q Q _________ `v & O
\ Ci i o ________ * 7 4
<o
lo o
____ ________
i?M
C - o w c ie i> - W 4 - 7 -^
(1) Millipede MllH-Qa lugli purity water T<ts
00708
ENVIRONMENTAL LABORATORY
lr
OECD ACTIVATED SLUDGE RESPIRATION INHIBITION TEST #209
f t 1351 6 o J f S'
RAW DATA
Test Substance: 3 . 5 ~ Q nc K \ chT o ^ W e ^ c > l____________________________
Source of Activated Sludge Mixed Liquor: N \ ^ ro ld g s \e , Date Received: 3 ~<3 t
_
Date Used: ^ - 2 7 r 9 7
Analyst:
*"T ^ 5 __________
5 -V.Pq ^
30-MINUTE EXPOSURE
Test Substance Concentration (p^ I l.) 0.5
1.0
DISSOLVED OXYGEN CONCENTRATIONS, mg/L
TIME MINUTES 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0
Temp 5.5 C
BKCONTROL 1 to
7.4, 7 .3 <*n 6 . 2 S -V SM 7 -7
3.7 3 .2 2.S
B .X
7 -6
6.7 6 7
6 : 9 G-C5 5-7 S H 5 . 0 f l / . o --
1
BKCONTROL II
S.l 9.6 7 - x 3,7 3 3 7 * 4 '7
/ o 0.4, a i.o
3-HOUR EXPOSURE
DISSOLVED OXYGEN CONCENTRATIONS, mg/L
Test Substance
TIME - MINIITES
Temp
Concentration (n ^ lt) 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5
c
BKCONTROL 1
to
7 S.S
7 * 7-S 7 .6 fc-S 6 4 5 .7 S 3
19.2.
* 7 7 ? ?.S S.M ? .x * .o 7 t _ 7 .S 7 M 7 . X X o . i
-- --
BKCONTROL II
7 .7 l.(o 7.2- <*s 6 2 , 6 7 S S S-f
4-3
pH of activated sludge mixed liquor: pH of highest concentration tested: Test temperature: *7.3. - 2 f-G
Initial 7 - 7 ______ Initial Sr-o
Final ^-6 Final * 7
3 .^ X A 3
002705
<002-7 dbO
L Ed
ENVIRONMENTALLABORATORY
CALCULATIONOF RESULTS.; ' 1 *(--r 1! ;.J i i- S ' 1 Test Substance: 3-5-Oichloroohenol Analyst: Trudv Stiefenhoefer
O EC D Activated Sludge Respiration Inhibition T e s t #209
Lr. R13ai Date: 3 /2 1 /9 7
30-Mlnute Exposure
mg/L 0.5 1.0
2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5
R
% lnK (3|
A
d
h
P ^ II^ tw ll
BK1 7.6 7.3 6.7 6.2 5.8 5.4 4.9 4.2 3.9 3.2 2.8 21.6 0.9915 0.8871
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 0.6303 0.5880 32.0
t
BK2 5.1 ) 4.6 4.2 3.7 3.3 2.7 2.4 1.9 1.4 1.0 0.6 21.0 0.9018 0.8412
% diff in controls (4): 5.3
FlaCm (5): 0.8642
3-Hour Exposure
[
rng/l
0.5' - 1.0 X S 'V
I - v "
I `
B M s ii
V > s- v V>
BK1 9.0 8.7
10 9.0 8.9
1.5 I
8.5 8.8
Dissolved Oxvijen Concentrations, mg / L ____________________________________________________
2.0 I 2.5 I 3.0 3.5 4.0 4.5 5.0 5.5 Tamp, *C I R (1) Ra (2) %
, A> A , >V ` | w ! " ^
l iiil
W m m m M iilllliM
8.2 7.8 7.5 7.0 6.5 6.1 5.7 5.3
19.2 0.7891 0.8342
8.5 8.4 8.2 8.0 7.8 7.5 7.4 7.2 20.1 0.3891 0.3864
lnh. (3) 53.1
I
BK2 7.9 7.6 7.2 6.8 6.3 5.9 5.5 5.1 4.6 4.3 3.9 20.3 0.8315 0.8144
% diff in controls (4): 2.4
RaCm (5): 0.8243
(1) R- Oxygenuptakerat(mg02A.-mh)
(2) Ra Requatedto20*0 [R/#.Ex|
(3) % Inhibition [(RaCm)-RaS/(RaCm)]100
(4) %dttetence incontrols: [IRaBk1-RaBk2l/RaCm]100 (Two controls must bwithin 16%(4 aach other.)
(5) MeanadjustedR, control# [Ra8k1+RaBfc2]/2
a> 1.072
Bka blankcontrol, S sample
x Tobs-20*C
RaCm meanadjustedR, controls
Tot sampletemp
NaOH Total Containers o f Each Hem
002711
I8L 203
V Si ri
\ n M
Ll-- 1-7 - E >,
Chain of Custody Record
3M Environmental Laboratory
Fom 35176 - PWO
P \
Address
"
City, State, Zip Code
w - * cm.-.-
3M Project Title
" 3M FedUly Contact
3M Telephone Number
07659
SMRequetter 3M Project Lead
U t,
u
I ! 'J" - ,, ,,
....1
3M Project Number
U Y
3M Department Number
\/w
Lab Requesremplate Number
Sampled Br (Print) \
MU
fe Z
jL
Item
#
* Sample Description
1 jf c d L
2
Du <l v . \ l
3
4 5
6 7 8
9
10 11 12 13
Item #
Number Containers oteach
Preservatives
Sam ples Split See Attachm ent Comments
Date Time Matrix
1
2 M rj0 ^ ^ 1*
lk < - >
n
ii
o
z
z
V
8M
X
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Time
Date
3p j n -
Shipped Via
5E
ecelved By/Affiliatlon
Time
Date
zS'. 13 ' b f h '
Original Accompanying Samples
Last Page - Orignator
See Reverse Side For Instructions
