Document zQoNmKvwNKnB5DaOB9eepy5z0
Evaluationof RespirationIn and BOD/COI sheets (Lisalt
ACTIVATED SLUDGE RESPIRATION INHIBITION TEST
TEST SUBSTANCE
Identity:PerfluorooctanesulfonatLei,thiumsalt;may alsobe referredto as PFOS Lisalt,FC-94, or FC-94-X. (1-Octanesulfoniaccid, 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecaflliutohriou-ms,alt, CAS # 29457-72-5)
Remarks: The testsample isa mixtureofthe testsubstance inwater (approximatel2y4.5% testsubstance and 75.5% water).No calculations were made toadjustfortheactualconcentrationofthe testsubstance in the testsample.
METHOD
Method: OECD 209 Test type: Staticacute GLP: No Year Completed: 1994 Analyticalmonitoring:pH and DO concentrations. Statisticamlethods: Not performed Test organism source:Activatedsludgemixed liquocrollectefdrom the MetropolitanWastewater Treatment Plant,St.Paul,Minnesota.
Test conditions Dilutionwater: MilliporMeilli-Q@w)ater Synthetic Sewage: Per OECD method Reference and testsolutionpreparation:A stocksolutionofthe referencesubstance,3,5-dichlorophenolw,as prepared per the OECD method. The pH ofthe referencesolutionwas measured to be 7.4. The testsolutionswere createdby directadditionofthe testsample;finalconcentratioonf 1000 mg/L. InitiaplH ofthe two 1000 mg/L testsolutionswas 7.1and 7.2. Test vessels: One litegrlassfleakers. Number of concentrations:1 (done induplicatep)lus 1 reference controland 2 Blank controls Temperature: 14.7-16.80C Total Suspended Solids and pH forsludge on day of testing: TotalSuspended Solids= 4.9 g/L (mixed liquor).Finaltestsolution mixed liquorsuspended solids= 1.92g/L. pH oftheactivated sludge mixed liquorgave an initiraeladingof6.4and a finalreading of 6.7. Element Basis: Respirationinhibitioans determined by oxygen consumption.
MethodRemarks:Dissolvoexdygeninthetesstolutiownass quitleow duringthe30-minuteexposureportionofthetest.The technicianrealized thetestreactorswere notbeingsufficientaleyratedafterthe30-minute readingsand adjustedtheairflow.Because the3-hourdata isthemost commonly used data,itwas decidednotto re4estdue tothisoccurrence.
Test temperatureswere notcontrolledduringthetest.The respiration rateswere normalizedto200C forthecalculations.
RESULTS
Nominal concentrations:Two Blankcontrolso,ne referencesubstance (10mg/L 3,5-DCP),two 1000 mg/L testmatedalsolutions.
AnalyticalMethodology: Analysisof DO concentrationisnalltest solutionswere performedusinga dissolvedoxygen meter.
Control response: Satisfactory
Remarks: Values reportedareforthetestsample. No calculationwsere made toadjustfortheconcentratioonfthetestsubstanceinthetest sample.
CONCLUSIONS
The testsample containing24.5% PerfluorooctanesulfonaLtiet,hiumsalt exhibiteda maximum inhibitoerfyfectof35% upon respiratioant a nominaltestsubstanceconcentratioonf 1000 mg/L at3 hours exposure. The 3-hourEC50 (respiratiionnhibitioins)>1 000 mg/L.
Submitter: 3M Company, EnvironmentalLaboratoryP,.O.Box 33331, St.Paul,Minnesota,55133
DATA QUALITY
ReliabilityK:limischranking2. Thisstudylacksinformatioonn the sample puritya,nd thetestwas conductedattemperaturesbelow those recommended by themethod. Oxygen concentrationaslsowere toolow to allowan adequate measurement of oxygen uptakeratefollowintghe30minuteexposure portion.These 30-minuteresultwsere considered invalifdorthestudy.Itwas concludedthat,sincethe 3-hourresultshow acceptabletoxicittyh,e30-minuteresultsalmostcertainlwyould have shown thesame.
REFERENCES
This studywas conducted by the 3M Company, Environmental Laboratory,Lab Request number Ml 018, 2/22/94.
OTHER
Last changed: 5/3/00
EVALUATION OF FC-94-XBY OECD ACTIVATEDSLUDGE RESPIRATION INHIBITIOTNEST #209
Results
,TheinhibiteofrfyecotfFC-94-Xt,helithisuamlotfperfluorooctanesulofnonate, activatseldudgerespiratwiaosnevaluateudsingOECD Test# 209.After calculatteedmperatucroerrectiomnesa,surementfsollowian3g-hours exposurteoFX-94-Xat1000mg/L,showedactivatseldudgeoxygenuptake ratewsereinhibitbeyd34%.Thereferenscuebstanc3e,,5-dichlorophaetnol, 10mg/Lcausedaninhibitoifo5n6%.
Discussion,
Thoughthistudyhaddeficitthse,analysctonsidetrhsatheresulatrse sufficiteonatssessthepotentifaolrwastewatetreatmesnytsteminhibitbiyon FC-94-X.
One studydeficwiatsthatoxygenconcentratiwoenrsetoolowtoallowan ade.quatmeasuremenotfoxygenuptakeratefollowitnhge30-minuteexposurpeortionftheOECD #209studyT.hese30-minutreesulatrsethus invalainddshouldbeignoredT.he 30-minutresultasrenotcrititcoatlhe usefulneosfsthestudyh,owever,becauseinhibitiisaolnmostalwaysgreater followi3n-ghourosfexposureI.fthe3-houresulsthsowacceptabtloexicity, the30-minutreesultaslmostcertainwloyuldhaveshownthesame.
A seconddeficiisthatemperatucroentrwoals notused.Measuredtest temperaturweesrelowerthanthatrecommendedbg'thmeethodbyasmuch as 5.5OC.However,altlestwsereconductewdithi1n.5degreesofeachother. Also,priotrocomparisoonftheoxygenuptakeratesc,alculatiwoenrsemade toadjusttheratetsothoseliketloyhaveoccurreadt20 OC. Theadjustment usedwas theruleofthumbthatmetabolircateosfmesophilmiiccrobial populatiotnyspicaldloyubleforeach10OC Increasientemperature.
July22,1998
,JNTERNAL CORRE,SPONDENCE13M
TO: ERIC A. REINER FROM: SUSAN A. BEACH SUBJECT: Review ofOECD 209 and BOD/COD TestResultsforFC-94-X
DATE: July8,1998 Ihave reviewedthe resultfsromthetestof FC-94-X on theinhibitiofnactivatesdludgerespiratioinhibition (OECD 209) and have a few comments. 1 . Althoughthe dissolvedoxygen inthetestsolutionwsas quitelow duringthe30-minuteexposure portionofthe
test,itwas adequate after3-hoursexposure.The techniciarnealizetdhetestreactorswere notbeing sufficientaleyratedafterthe30-minutoreadings,and adjustedtheairflow.Because the3-hourdataisthe most commonly used data,itwas decidednottore-.tedsute tothisoccurrence. 2. At the timethistestwas run,thelaboratordyidnothave a procedureinplaceforcontrollitnhgetemperature duringexposure. The temperatureofthetestreactorsfluctuatewdiththetemperatureinthe hood. Because thiswas testedinFebruaryinMinnesota,itisnotsurprisintghatthetesttemperaturewas so low. The respiratiornateswere normalizedto2(rC forthecalculations. 3. The softwareused toproducethe datareductiosnheetsdidnot have an easy way todepictexponents,so the equationforthetemperature-adjusterdespiratiroantes(Ra)isdiffictuoltunderstand.Itisas follows:
Ra = R adjustedto2CPC R x
Where 0 = 1.072 x = T (observed)-200C
if
4. Even though the 30-minutedataisinquestionand thetestwas conductedatlowerthannormaltemperatures, the data are usefulforthe interpretatioofnthetoxicitoyfFC-94-X toactivatesdludge.An average of34% inhibitiwoans seen at1000 mg/L. We generalldyo notconsiderinhibitiloenssthanor equalto 15% to be significawnhten usingthisprocedum due tothe inherentvariabiliotfythe method.
As forthe BOD/COD testingw,e have been unabletolocatethe dataatthistime.
Pleasesee me ifyou have any questions.
Regards,
Susan A. Beach
ENVIRONMENTAL LABORATORY ACTIVATED SLUDGE MD(F-DUQUOR
LR
Date ;?t@t;)Ily Analyst Page I of 14
Type Test: OECD ACTIVATED SLUDGE RESPIRATION INHIBITION, 209
ACTIVATED SLUDGE MIXED LIQUOR
Date Obtained
Date Used
Mixed Uquor Suspended Solids(MLSS)
g/L
MLSS infinaltestsolution
g/L
InitipaHl (p,q (Isttestsoin.prepared)
Comments
Adjusted'to FinalpH (o,
g/L (lasstoln.prepared)
TEST SUBSTANC Sample DescriptionFC-:-CJLI-Z InitiaplH of highestconc. tested Comments
-7@.R
AdjustedtopH
REFERENCE SUBSTAN
Sample Description
%C\ALLRCEZ:beApl-
InitipaHl of stocksolutio(n';;00 mg/L)-
Comments
'Adjustedto pH
EXPOSURE CONDMONS
Test Duration
'V@a3@?-S
Test Temperature Range:
14.
Comments
t,, c
LR ENVIRONMENTAL LABORATORY OECD ACTIVATED SLUDGE RESPIRATION INHIBITIONTEST #209 TEST SOLUTIONS PREPARATION
Test Substance: FC- - 9 Lt
Sample Description: Analyst: Date: ,7@
o%-@- LA
Test Conc. mg added
matl
12er500 mL
mL MO(l) water per 500 mL
mL syn.sewage feed 2er 500 mL
L
mL microbial inaculum oer 500 mL
TotalVolume mL
/COO
m
Zq
-ZjzAfz@i/gy
COA)CITc--,T-
)AIJriAL
Sol,, @ilu
tocx)
(1) MilliporMeilli-ORhigh puritywater
ENVIRONMENTAL
LAIBORATCRY
OE",D ACTIVATED SLUDGE FiEc-PIRATION INHIEITICN TEST 9209
RAW DATA
Tes,elSubs-,,ance:
9 4-X
Source of Ac#4,ivaStie'dudgeMixedUquor:hit, Ul,-,TaE@-keTreqir,,Ps,,li
DateRec--zived: I-CIL(
DateUsed:
Analys,
30-,MINUTE EXPOSURE
TestSubs=ce Concentration O@it
DISSOLVED OXYC-@r-NCONC=Nrir--.A-i]CNS, mg(L
TIME-MINUTES
1.0
2.0 2.5 3.0 3.5 4.0 4.5 S.o
Temp cc
F-KOCNTRCL I
q.0
b,ci
110.9 1r Io.<,-I - I- I I
SK CCNTRCL 11
9.0 1-7,-717-q 1-7.1 (@,g
S"9
3-HOUR EXPOSURE
Dr,-Z-@OLNr=-ODXYC-r--N CCNC-=NTr--A-iICNS, mgtl
Ie--tSubs=ce Concentration m-KCCNTRCL I
/6-C
TIME - MINUTES
Temo
0.5 1.0 1.5 2.0 2.5 13.0 3.S 4.0 4.5 5.0 =.S
cc
I
I
I
I
I
(o i7,V -7,1 -3 G-0
6,3 5-,!g15,3 15.1 1q,g
lq,5- 1(
15.3 S-..l11419 q. 114I.r lq,3 Iq.1 13@@ 3.+ 135- 13)3 I-
-=K C*--dNTRCL 11
,:,-Hof ac*.ivated sludge mixed liquorcH Of highest concentrationtes,,ed: @est temperature:
Initial Gq
Initialti,
S.-7
F:;nai(@o,
F'nal t.,S'
Z4.(10 Li,g
ENVIRONMENTAL LABORATORY OECD ACTIVATED SLUDGE RESPIRATION CALCULATION OF RESLA.TS
INHIBMON
TEST #209
Test Substance: FC-94-x
Analystf:M
30-Mlnuto Ex)osure
Dissolvd OxyCen Concentrati s,mg/L
/L 0.6 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5..0O0@ 5.5
BK1
7.0 6.9 6.4 6.0 5.7 5.4 5.0 4.7 4.3 @ 4.0 3.6
looo.o 2.3 1.7 1.5 1.2 1.0 1 0.8 0.5
1
1
iooo.o 1.2 0.0 0.6 0.5
T -C R (1 16.6 0.707 16.8 0.474 16.8 0.400
BK2
8.0 7.7 7.4 7.1
% diffincontrols(4): 10.1
6. 1 6.5 6.2 5.9 1 5.6 EC50 (96% Cl):> 1000 mgtl
5.4 J_ 5.1
3-Hour Exposure
Dissolv d Oxycen Concentrati s, m cov/
/L .0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.6 5.0 5.5
BK1 7.9 7.6 7.4 7.1 6.8 6.5 6.313 6.0 5.7 5.4 5.1
iooo.o 1 6.6 6.3 6.0 5.9 ;5.7 5.5 5.33 5.1 1 4.9 4.7 1 4.5
iooo.o 5.3 5.1 4.9 4.7 4.5 4.3 4.1 53.9 3.7 3.5 3.3
15.2
Tamp. OC
14.7 16.0 15.9
0.580
n (1)
0.558 0.391 0.400
BK2 1 7.4
1 6.9 6.5 6.2 6.0 5.7774 5..40019-1 5.2 4.9 1 4.6
% diffin controls(4): 2.3
EC 60 (95% Cl):> 1000 mci/L
14.9
(1) Ro Oxygen uptake rate(mg 02&-ndn)
a- 1.072
(2) Ra- R adimied to
IRI@."
R&Cm- mean ad*ted R. mdmb
(3)% lnldbkki)(mRaCm)-RmS/(RaCm)lloo
Bk-blanckontrSonls.ample
(4)% dnioreinncceortroIlIsR:&Bkl-RaBk2VRa(CTmwlocloonotrmoulsstbewkhl1n6%oleacohther.)Tobs-samplteomp
(6)MeanadjudeRd.coriro[bR=aBkl+RaBl2y2
x-Tobs-20*C
0.553
ENVIRNOMENTAL
LABORATORY
OECD ACTIVATED SLUDGE RESPIRATION INHIBITION TEST#209 TEST SOLUTIONS PREPARATX)N
Test Substance:
Sample
Description:
@RoA
Analyst:
I
L-nbp\ tc, i-,Ajo
Date:
Stock Solution
Preparation::-
IL-
A scn,
A b-oM --r@ U\JrFn -@n_
k-D -Li ri-7ft 0%_@H -7,q
L MQ u:bTE(Z
or-3.
Test Conc. mg/L
mL added 12er500 mL
mL MO(l) water 22r 500 mL
mL syn. sewage feed 12er500 mL
mL microbial inoculum per 500 mL
TotalVolume mL
ID
-7Li
(1) MilliparMeilli-ORhigh puritywater
ENVIRONMENTAL
LABORATORY
OE--D AC-nVATE-:) SLUDGE RE-FIRAI-ION INHIBITION TEST -209
RAW DA i-A
Tes*L Substance:
Source of Ac#*IvatedSi'udge Mixed Liquor:
Date Re---cived:
L(
Analys,
@@l +
T- ST, Pl
Date Used:
30-,MINUTE EXPOSURE
Test Substance ConcentrationQ%jtL) 0.5 1.0
F,KCONTRCJ- I
I- 1
DISIZCLVED OXYC-=-.NCONC=NTRA-iICNS, mg(L
TIME-,MINUTES 1.5 2.0 2.5 3.0 3.5 -4.0 4.5 5.0
Temp S.c CIC
5;q 14,-@-14.3 1L40.
-7,7 -7,9- 1-7,3 17, cZ 17.6
. ......................
'3.(o1/(Olb
EK CCNI FICL 9
1
3-HOUR EXPOSURE
ENSSOLVE-:) OXYC-=N CCNC=NTm-A-iICNS, mgl-
Test Substance
TIME - MINUTES
Temo
ConcenWation (MI/L 0.5 1.0 1.5 2.0 2.5 13.0 3.5 4.0 4.5 C.0 5.5
SK CONTRCL I
,-1.9 1,6 7,q -7,1 1(o.,? (0,
(o,C)!5,
I!&,). 31 1 3@D
7,cl 1-1,1 @7. -1 1-7,S-, q -7.3 -7.R '110 liq,or-
P-K C'-.N-Md C.L U
7,q [-7,J
P-oHof acoivatedsludge mixed liquor: Initial *pH of highestconcentrationtested: Initial (a Test temperature:
Final F-nal (@o--7-
EWIRONMENTAL LABORATORY
OECD ACTIVATED SLUDGE RESPIRA71ON INHIBMON TEST #209 CALCLLA11ON OF RESULTS
Test Substance: 3.5-Dichlorol2henRoelferenceSubstance
Analystf:lff
30-Minuto Ex osure mg/L 0.5 1.0 1.5
n
BKI
7.0 I 6.9 6.4
10.0 8.6 8.4 8.3
Dissol d Oxycon Concentratis,m 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5
F.. 6.0 -5.7 5.4 5.0 4.7 4.3 4.0', 3.6
8.1 7.9 7.7 7.5 7.3 7.2 7.0 6.8
To -c R (1) 16.6 0.707 14.7 0.363
7.7 7.4 7.1 1 6.8 6.5 6.2 6.9 5.6 1 5.4 5.1
% diffincontrol(s4): 10.1
ECSO (95% Cl):> 10 mgll
3-Hour Exposure
Dissolwdv Oxyten Concentratis,mg/
/L .0.5 1.0 1.5 2.0 2.5 3.0 1 3.5 4.0 4.5 5.0 5.5
BK1 7.9 7.6 7.4 7.1 6.8 6.5 6.3 6.0 5.7 5.4 5.1
10.0 8.2 8.1 8.0 7.9 ,7.8 7.7 7.5 7.4 7.3 7.2 7.0
15.2
Tww. oc 14.7 14.5
0.580
R (i 0.558 0.241
BK 2 7.4 7.1 6.9 6.5 6.2 6.
1 5.4 5.2 4.9 4.6
% diffincontrol(s4):. 2.3
EC 50 (95% Cl):< 10 mgll
14.9 1 .553C
(1)R- Oxygenqmam rde (mg02&-Wn) (2)Ra- R acQM*d So20-C- Pe.Exi (a)% inhn*bn-i(R&Cm).Ras/(Racm)lioo (4)% dn[wonceIncoraralsI:lRaBkl-RaBk2MaCm]100(Twomdmb (5)Mom adoged R.wi*obu PUMI+RaBk2y2
mustbe whmn 16% ofeachothw.)
1.072 R&Cnv- mean adlmlodR,mdrols Bloxblanmkdrol,Sm umple Tobsu sampletamp xn Tobs-2010