Document 6BkoLREd4QGoReRnpBxQmeG9E
BIODEGRADATION (BOD/COD)
TEST SUBSTANCE
Identity:A mixturecontainingperfluorooctanesulfonatew,hich may also be referredto as PFOS, FC-95, or as a component of FC-600. (1-Octanesulfonicacid,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8heptadecafluoro-,potassium salt,CAS # 2795-39-3)
Remarks: The 3M productionlotnumber was not noted. The test sample isFC-600. Current informationindicatesitisa mixtureof 1.0% PFOS, 81.20% water, 12.00% diethyleneglycolbutylether,1.00% sodium octylsulfate,2.00% propane Sultone foamer, 1.00% sodium decyl sulfate, 0.85% xanthan gum, 0.1% N-(3-chloroallyhle)xaminium chloride,0.80% starch,and 0.05 % tolyltriazole.
The following is an abbreviated summafy of multiple biodegradation studies on FC-600. These studies apply to a mixture with incompletely characterized concentration of impurities. Data does not accurately reflectdegradation potentialof the fluorochemical component of the testsample.
METHOD:
Methods: OECD 301 E and BOD/COD/TOC (summary listinognly) Type: Aerobic GLP: No Yearcompleted: 1975, 1983, 1984, 1988 Contact time: 20 days (BOD) and 28 days (OECD 301 E) lnoculum: 1984 studyused a 50/50 rviixtuorfesoilextractand secondary effluent.Sandy loam soilsobtainedfrom Ramsey and Washington countiesin Minnesota. The secondary effluentsample was supernatantof activatedsludge mixed liquortaken from the Metro Wastewater Treatment Plant,St.Paul,MN. lnoculum forthe otherstudies was not noted.
RESULTS
Chemical Oxygen Demand: BiochemicalOxygen Demand
(BOD): 5-Day: 11 -Day: 14-Day: 20-Day:
467,000 mg/L*
50,000 mg/L* 255,000 mg/L* 240,000 mg/L* 237,000 mg/L*
Data was availableas a summary lisotnly. TotalOrganic Carbon (calculatefdorthe product): 0.097 g/g
TotalOrganic Carbon Removal:
90 - 91% in28 days
DissolvedOrganic Carbon Removal: 79.9- 94% in28 days** ** Range over 3 separateOECD 301 E studies
Remarks: Testingwas conducted on the mixtureas describedintheTest Substance Remarks field.The value reportedappliestothatmixtureand not the fluorochemicalproportionalone.
CONCLUSIONS
No reliablceonclusionscan be derivedfrom thisstudy. The indicatioins thatthe majorityofthe productcomponents are readilybiodegradable.
Submitter: 3M Company, EnvironmentalLaboratory,P.O. Box 33331, St.Paul,Minnesota,55133
DATA QUALITY
ReliabilityK:limischranking3. The inoculum isnot properly characterizedinmost studies.The testiiiwgas conducted on a mixture withchemicals havingvaryingdegrees of biodegradabilitlye,adingto potentiamlisinterpretatioofnthe results.The sample puritywas not properlycharacterizedand the studylacksanalyticaclonfirmationofthe amount offluorochemicalproportioninthe solutions.
REFERENCES
Testingwas conducted by the 3M Company, 3M EnvironmentalLab, St. Paul,MN, Lab Request Numbers 2874 and 8483.
3M Environment Assessment inquiry#82326, E.A. Reiner,3M EnvironmentalLaboratory,St.Paul,MN, April21, 1983
3M TechnicalReport "OECD BiodegradationTestingon FC-600 and FC203."E. A. Reiner,Project9972410100, 3M Germany, Report Number 001, April18, 1983
3M TechnicalReport "ModifiedOECD ScreeningTest on FC-203, FC203A, and FC-600."E.A. Reiner,Project9970010100, International, Report Number 003, July9, 1984.
OTHER
Last changed: 6/28/00
Fo,rn 10620-5-PWO ca: LAB REQUEST
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PRODUCT ECOLOGICAL ASSESSPAENT
REOIJEST FOR LABORATORY
WORK
DIVISION
LABREOTJESTNO.
Name: Reque s"t Date: ProjectNo.
Code No: Sample Date:
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70 3
Desr;ription: Purpose of I ests
REOUESTFR
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LABORATORY Atti')Iilb
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Hours Spent:
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PHYSICAL & CHEMICAL PROPERTIE Heat of CornbustionCal/G IBTU/Lb.) Density Ash Othe(
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SAMPLE FORt4 SHEET FOR IME MODIFIED
Exp. no.: Date Of start of to t: TeAt * '-@t'andarLd-at:rial! Theoro-ti@-I -Cst conc.: inoculus: Carbon analy*er:
OECD SCREENING on DOC-/I
TEST
A: Cont_tgll:
I TOC* I DOC**
1M-0-cW 307u=on of the test material
i(lo ,o , dilution
I
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8: Carbon date @rminetions:
I
.
I
I I Culture nedi,
1I1n"Loos.mi
minour nutrient;
@ sol tiaoln with
Itest mater=a
1
land with
I
linoc-utu-s
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lyses I6
IThear. I DOC - concentrations -aTce-r-x-rsy-sI
Iconc. I
mg/l
mg/l 0 (CO) I-a 71
I 141 .,221v 271 28 1
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1
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el
lsolution withoutli3lankl
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ltest note-rl-al-l
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I
I- C2 I
Iinocu-rui-a
I
I-
I
I
cl C21
1
1-3
I
I(Cbl)
I
I
Disagreement between DOC and TOC values points towards of the test material.
All DOC values determined after membrane filtration.
insufficient solubility
@/2
2
"Ready Biodegradability: Modified OECD Screening Test,#
1
C: Eva:uatlon
of raw Ogta:
IFI@Bkl lno.
ICXX - concentrationsl
Ininus
Iblanks
I
I
I
IDI
mit 03t 01
2 1,,@
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mean ID
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1
2
I f-o day x
remove
or
1 71 141 211 277 :yesI
100 1
ino I
"Ready Biodegradability: Modified OECD Screening Test-,
301 E
I Page 11
ANNE X
SAMPLE FORM $MEET FOR-IHE MODZFIED 0
Exp. no.:
Date of start f tea TeAt * '-@tandardestarialt
Theoroti^t! Inoculun:
tc3@. L:onc.:
Carbon a.iaiys
R.EENING TEST
A: Control3:
I TOC* I Doc** I
of tht tea mate al
go/I. dilutin.
tolutlon) I
8: Carbon determinations:
1:77C- 2-
I Culture o dium I 1
IMine I nutr
Isolution with
Itest mate-rTs-T
land with
Ii nocu=um I
lno. I 1 I
2
'_'J'
I 1
lco'nc. 1 49/1 1
DOC
concenEr-arro-ns--aTre-r-X-Us-y-51
I
g/l
10 (co)l.4--@,71 -.1141,v2llU271
f
1 28 1
1
82
I
I
1
--7
1 01 + 021
jol
I(Ct)
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7--7-1
1
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1
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I
bl
b21
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I(ct)
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isolution without Slankl
cl
ltest mote-rT-41-
lbut with
C2
nocu"M
I-
Ir
cl + C2
I 03 le 1
I(Cbl)
-76. 10
Disagreement between Of the test materiel. DOC and TOC values
points
towards
All DOC values determined after ambrans filtration.
insufficient
solubility
FC- 60@
/12 12
"Ready Biodegradability: Modified OECD Screening Test,,
C: Ey
or raw ci4t*:
IDOC - cOnCentrational lmlnus
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irioI
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1
1
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1
1
1
"Ready Biodegradability: Madifie d OECD Screening Test-,
301 E, IPage
NNEX
SAMP@E FORM-$,MEET F R IHE MODIFIED OECD SCREENING TEST
Exp. no.:
Date of start of to t:
TeA@ * 'Oendard L-st:ria- -r! Theoroti@.1 '--3t L:Onc.: Inoculum:
mn DUC77
Carbon
A: Control$:
I TOC*
,@'U@K
3o.Lu,.ion of the-E-e-sTmateriaT-1
1000 mg/l, d ilution
.../1000 ml
8: Carbon determinations:
DOC-* I
I
lflaski Analyses
I Culture medium Ina. I I
1
IMineral nu-E-rT-ent,
Isolution with I
Itest mater=a
1
land with
I
linocu=ua
I
I
I
1
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ii
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71.,o
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g/l
71 1
I 1 211 2 71 28 1
-7----r
1
1
1
3
.2.-7
/,7
13.1 1 2..l
Imineral nutritnti
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. IL3K
linocu=um
'C' c2
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1
Ile -Y, 11io@-- on-w "All
*!.,Oil
cl + C21
I
l(Cbl)
-0.101
os
I
I
I
Disagreement between DOC and TOC values pointo towards of'the test material.
All DOC values deterained after membrane filtration.
Insufficient solubility
"Ready Biodegradability:
M"
Modified OECD Screening Testle
1'/l 122
C Eva:uation of raw data:
IFlask
Ino.
I
IDOC - concentrationel
lninus
I
[I blanks
I1 1 IIDI
sit 143t 03
22
m2t - 03t f-2- 03
lneen 10
Dl 02
2 r-or.dayx
100 lrbo
1
Fc-- coo
remove
or
71 141 211 277 a2yes I'
I
1 7-1
Form 6747-11 -E
TECHNICAL REPORT SUMMARY
TO: TECHNICAL COMMUNICATIONS
CENTER - 201-2C-12
(linportan-t Ifrc@poritsprintedon both sidesofpaper,send two copiesto TCC.) Guidelineson reverseside.
Division 3M 1,nv i ronmc
3M Get,.@many
Roport Ti
n ti I La hora tory
( PC & PC) S t . Pau 1 Mi nnesota
Dept. Number
0535 Pro@octNumL)or
9972410100 Report Numuor
OECD To
Biodegradation
Testing
K. F. SchrQeder, Au thorls)
!@ E. A. 'I'l@einer, Notebook Reference
3M Neuss, Environmental
on FC-600 Germany
Laboratory
and FC-203 - 21-2W-05
Period Coverou ur @aLe
4/18/83 Employee Number(s)
47816 No. ofPagesincludingCovershoot
None - See 3M Environmental
Lab Request
8483
15
SECURITY 10- 00nenRooort&Summarv
[]ClosedReport-Open Summary
3FACHEMICALip, REGISTRY-
KEYWORDS: Lai)Code
CURRENT OBJECTIVE:
1. To products
measure using
the biodegradability the internationally
OtlierKeyvvords
OECD Screening
Test.
Check box ifnew chemicalsarereportedU.se Chem i Xcal RegistryForm 6092 toreportallnew substances,
of two recognized
"Light
Water"
Modified
2. To compare
using
the same
results
with
test method.
those
previously
obtained
REPORT ABSTRACT: Thisabstractinformationisdistributebdy theTechnicalCommunications Ceritetroalert3M'ersto Company R&D.
This
study
used the Modified
OECD Screening
Test with
dissolved
organic
carbon
(DOC) analysis
to measure
the
biodegradability
of "Light
Water"
Brand
AFFF
products;
FC-203
and FC-600.
In 28 days,
the DOC levels
of FC-600
degraded parallel
by 80% and 92% for an average
of 86% in two
tests.
In 27 days
the DOC of FC-203
degraded
by
77% and differed
81% for an average
of 79%.
The FC-203
result
from a similar
test done in 1980 in which
93% DOC
degradation parallel
occurred
within
sterile
controls
21 proved
days. that
In the present the DOC loss
study was not
due to chemical
or physical
processes
such as adsorption,
volatilization,
or precipitation
of the organic
compounds.
InformL@tionLiais
FC-600/FC-203
P,ii(e 2 April 18, 1983
Introdtiction
The 3M Environmental Lahoratory underto(-)k thi.s study of the
biodegradability
of "Light Wator" I)roducts, FC-600 and L@'C-203, 1)(@(@ause
of concern cxLjross(-,d L)y 3M C,or-inaiiayl)oul inconsistencio.-, in L),If@l
biodegradation
test results.
Modified OECD Screening Tests conducted in 1980 by the 3M
Environmental
LAboratory showed that three "Light Water" prociuct!T@were
highly biodegradable.
FC-203A,
were shown to have 90% of their
the OECD Screerting Test. These
FC-206, and FC-3017 (FC-206 U) i.l.l dissolved organic carbon removed in results, however, contradict those of
H. Hellmann and D. Muller(l) usin@)a similar yet not identical Lest method, the TOC Degradation Test( . In their study FC-206 and
FC-3017 were found to have total organic carbon reductions and 8%, respectively, in 21 days. These low biodegradation
of only 6% results of
Hellmann, however, were also contradicted by hi.s own work. tlis BOD5/COD ratios for FC-3017 and FC-206 were 0.5 and 0.4, respecti-vely.
This showed that 50% and 40% of the theoretical oxygen demand expressed within only 5 days. These levels of biodegradation
was are cnuch
greater than the 8% and 6% TOC removals which he observed in the even longer (21 day) TOC degradation test. This is clearly an inexplicable
discrepa.ncy in his work.
Hellmann's TOC degradation results are also contradicted by BOD20/CC)D
measurements
made by the 3M Environmental
Laboratory and other
independent laboratories on 3M AFFF products.
Such results typically
show BOD20 values to range between 60 and 90% of the COD. For
exampi-e, a collection of such da;--aon 3 U.S. military specificatio;i
AFFF products made by 3M is shown in Table 1.
Page 3
TA131,F,,I
DOD, CAIZUONACEOUS UOD, ANL) COI) DA'I'A ON MIL-SPLC Al-@t,@L-'
BOD20
C-BOD
COD
BOD20
C-BOD20
Lab
(mg/kq)
(mg/kg)
(mg/kq)
COD
COD
FC-203C Lot 501
3M
580,OUO
600,060
730,000
.79
.01
740,000
Pace
800,000* 1
730,000*
810,000 730,000
Serco
440,000
440,000
737,000
.60
.60
Capsule
570,000
620,000
950,000
.6
.65
Galbraith
616,000
671,000
776,450
.79
.06
S & VI Seed
Galbraith
670,000
641,000
776,450
.86
.02
Knoxville
Average S. D.
575,000
594,000
782,000
.73
.75
85,000
90fooo
80,000
.12
.12
Calculated BOD's from different dilutions were very inconsistent. Pace agreed to repeat this work but inadvertently lost their repeated test results as well. We did not request a third testing nor did we include these values in the averages.
FC-206C Lot 502
3M
Pace Serco Capsule Galbraith S & W Seed Galbraith Knoxville
290,000
350,000 240,000 260,000 416,500
395,500
290,000
370,000 260,000 320,000 411,000
374,000
380,000 360,000 450,000 370,000 410,000 407,250
407,250
0.78
0.78 0.65 0.63 1.02
.97
0.78
0.82 0.70 0.78 1.01
.92
Average So D.
3M Pace Serco Capsule
325,000
338,000
396,000
.81
.83
0
57fOO
33rOOO
.16
.11
FC-780B Lot 501
240,000
230,000
320,000
.74
.71
330,000
250,000
250,000
350,000
.71
.71
210,000
220,000
287,000
.73
.77
240,000
230,000
360,000
.67
.64
Average St Do
235,000
232,000
329,000
.71
.71
17,000
13,000
28,000
.03
.05
FC-600/FC-203 Page 4 April 18, 1983
Methods and Materials
1. Procedure
'1'(-,sLingwa-@,
in accc)r(iziticw(i@lli Llic,01-"Cl)
testing of chemicals adopted May 12, 1981.
2. Chemicals
The reference material used was laboratory grade sodium hei)zoate (C7H5NaO2) F.W. = 144.11. A 30.3 mg sample of this compound was diluted to 1.0 liters with the nutrient solution described I)y the method to yield a theoretical DOC of 20 mg/l. The "Light Water" samples used were supplied by G. Piessens, E.T.S.L. and consisted of FC-203 and FC-600. Lot numbers were not provided. Nutrient Solutions of the "f,ight Water" L)ro(itictwsith DOC's of approximately 20 mg/l (based on calculations from the forMLilatiOll) were prepared by bringing both 527 mg of FC-600 and 153 mg (-)f @'C-203 to 2.0 liters with nulrient solution.
3. Inoculum
The inoculum was a 50/50 mixture of the soil and secondary effluent inocula each prepared in accordance with the OECD procedure. The soil used was fresh loamy sand garden soil obtained from White Bear Lake, Minnesota, and the water for the soil extraction was chlorine-free well water. The secondary effluent sample was the supernatant from an activated sludge aeration basin at the St. Paul Metro Wastewater Treatment Plant. The combined inoculum was passed through WhatmanO 54 filter paper prior to usage.
4. Sterile Controls
Replicate vessels containing 400 mg/l HgCl2 served as sterile controls for both test materials and the reference compound. The sterile controls were handled in the same way as the viable cultures.
5. Instrument
The organic carbon analyzer used was a Dohrmann DC-52A. Its sensitivity limit is approximately 2 mg of carbon per liter.
6. Sample Handling and Storage
The sample preservation method used was that prescribed by the TOC manufacturer. The method involved adding 1 drop of concentrated HC1 per 10 ml of filtered sample. This brought the samples to less than pH 2. The samples were then stored under refrigeration in vials with aluminum foil-lined caps. Dohrmann literature indicates that the method can stabilize potassium hydrogen phthalate, a readily biodegradable material, for several months.
FC-600/FC-203 April 18, 1983
Du(? to [)roblems with th(, sonf-,itivityof th(, TOC ln,)lyzc,.rn,i)ly
half of the samples were analyzed within a month after sampl..i.i)g. Following 4-5 months oE storage, all of the, siin[)lcswere
reanalyzed. Comi-)arisonoE the 'I'OC-inalyses dotie within I inoiii-ii with those done after 4-5 months of storage showed that ii-i()ii]@y
one stored sample had the TOC changed significantly.
This F-,@iinple
was discarded.
Results and Discussion
Table 2 summarizes the resul*ts of this study. Appendices 1 and 2
contain the actual data sheets and plots of the degradation as @l
function of time. Table 2 shows that the sodium benzoate referetice
compound was nearly completely degraded within 14 days. Degradat4on
of both FC-600 and FC-203 continued throughout the course of the
28-day test period without plateaulng. At 28 days the averige '1'()C
removal for FC-600 was 86% and at 27 days the average TOC removal for
FC-203 was 79%. The test procedure recommends that chemicals giving a
result greater than 70% loss of DO('-(within 28 days) should be
regarded as readily biodegradable.
These 3M formulated AFFF pro(lucts
are thus even more completely degraded than is necessary for a
chemical to be considered readily biodegradable.
TABLE 2
Biodegradation
(% DOC removal) of Sodium Benzoate, FC-203 and FC-206
Product
% Degradation at Day:
7
14
21
27
28
Sodium Benzoate Sodium Benzoate
Duplicate
94.4 92.3
94.7 96.3
93.2 99.6
93.5 97.7
94.5 100.0
FC-203 FC-203
Duplicate
37.4 43.0
59.2 54.6
68.4 66.0
76.7 81.3
78.0
FC-600 FC-600
Duplicate
46 47.2
63.5 67.1
73.5 80.2
82.1 88.7
79.9 92.1
*Sample discarded due to probable contamination.
The sterile control data in Table 3 provide further substantial evidence that soluble TOC loss from the test samples is not due to physical modes such as adsorption, volatilization, or precipitation. These samples were handled identically to the test vessels, except that they contained HgCl2 to prevenit microbial growth. At the end of 28-day test period, these controls contained all of the initial DOC.
FC-600/FC-203 Page 6 April 18, 1983
'FAliLl3"
Conclusion
Percent c)f Initial Product
DOC in Sterile Controls % DOC Remaining
at 28
iays
@'C-203
98.1
1,'C-600
101.3
The present study demonstrates that Light Water products FC-203 and FC-600 are "readily biodegradable" according to the recommended 70% DOC removal criteria of the Modified OECD Screening Test. FC-203 an(] FC-206 had average losses of DOC of 79% and 86%, respectively.
References
1. Dr. H. Hellmann and D. Muller, "Environmental Impact of Fir(-,
Extinguishing Foam Compounds (Umweltgefahrdung durch
Feuerlosch-Schaummittell)."
The study was carried out by the West
German Institute of Hydrology (Bundesanstalt fur Gewasserkunde), April 18, 1979.
2. D. Muller and T. Tittizer, "The TOC Degradation Test - A Process to Test Organic Materials for Complete Biodegradation (.Der TOC Abbautest - ein Verfa hren zur Prufung von Organbischen Substanzen auf Vollstandigen Biologischen Abbau)." Developed at the Bundesanstalt for Gewasserkunde, Koblenz, Z. F. Waser-und Abwasser-Forschung (1979).
3. organization for Economic Cooperation and Development, Guidelines For Testing of Chemicals, Section 301 E, Ready Biodegradability: Modified OECD Screening Test, May 12, 1981.
4. Dohrman DC-52A Operating Manual, 4th Ed., 1978.
Page: 7
Appendix 1
S. A N N C X
2le6E F(HIN SHEET FOR IHE_MOBIFIED
E:P.no.: Lg :0 4 q 13
D to of STO-rt or test.
L)@- D -7
4MM * Stoodard retiqrlal!
Theorpli@el tz4t vanc.:
lnoculum: tgc4))JDAAY
l@ft-
Cargan wetelyoor; D2kiK AAA.Mtj
QECD SCREENING TIST pin PIX
A: Contrgls:
I YOCO I Doc** I
btock solutifn-or the test a-s-Es-rlal
I (SOOO
/it dilution
I .../aIla ml of nMt
as Corbon(taterainoti9ns:
Culture sodium Inc. I
'5 (:)p
an4.Ly$o$ 1, 1
I LA M
Thear.i OOC - conc@ngrgZ&gn$
llcgnc. 1
69/1
00/1 10 (co)
71
141
1wrn-*-T-gr-n-UT-r1on t
I"Iution
test met
1
end yllh
snocu=um
1
42
I jai a
(Ct)
+ g2
z
-7(0
-
d 0. '7/1,?, /,Y
grrgg x ugyil 1
211 271 26 1
-7'Ti I
21
b2
Kinevel nutrient
solution
outilll
oteustt astowlit*i
1
I
bl
(Ct)
nki
1
*2
b2i
f
I-V 1,20. it1.2.ol /,V 10,to1,0,rl/,4-1
10. 1 o,y5 I I
II
0
IN3
1
1
owtvient -
solution
without
Slank
test asteriet-
lk* lah
93
01809100MOt
betweeft
ON OW TIC values
points
toward#
insufflgl@nt
gslwbility
of tfw test "toilet.
P41 ON values detm""d
arta samovo
fistrattee.
,AVeiRA4E
OF- 131,AIUICS'
jo@
Of-reR
x -PAys
0-35C,
"Ready biodegradability:
E
$4odified OECD Screening Test"
12
C; Eye: !atlo!l of row (Iqtu:
ski
Ir10!
IOM - concentrotionel lninus
lblanks
'it
'3t 3t
IX DX removal after x days I 1 141 211 271 28 1 1
lyyq1, 1 93.Ilq,y
f-2 *3
lseen I
1
10
Di + 02
for day x
ino I
I
I
I
I
I
19.2.3 ; q
419 7
11,3 1 a I ilk 117 1
##Ready UiodegradabiliLy:
9
Modified OECD Screening Test-'
301 F-
IPage 11
.li A N N f X
C,AW@LE FOII14 SIILET FUI( IIIE_HOOIFIEU UCCU SCREENIK
TEST
Exp no,. @-)Qit194 9 z
Date or,,.tortof test:. 10- @-7-
-tondard L-.etmrial:
1--:@ tzz;'.:onc.:
inoculu
L;aroon
bnH 2 F.I4Lm ki
cA
inn I)M@
A: Contrgl
I TOC, I DOC** I
15tock solutioitof the test material I
1(1000 a /1, dilution
I
I
1960 Mi of nutrlgf)trolution) I
I
filaki
Analyses
I Culture sodium I no. I
lYhoor.1 DOC - concentrations after x
Icanc. I
mg/l
109/1 10 (Co)l-U71 4w 14140211 &U271 28 1
Igrn-o-r-a-l-n-ru7-ran t
olutt n ljlh I
I$test molter-re-T 1
42
land with
I
1I
linecu=uo
I
I-
I
al + 821
1
I(Ct) I
2
q, I
1
1
1
1
1
1
/ll,oI
I
III
I
q, 'IT. q,,q
I
bl b21
I (Ct)
Mineral nutrienti
solution9+rta@Wifilen kiI
a'
ltest set
I
C2
Iglut
llnocu"u.
I
I
cl + C2
113.'3
t
tj
4@l
L.
t?J
i
I
(Cbl)
-4-4
iffn-o r-lir hy & r a on t I
al
solutiez Without slwmkl
test as
wt
al + at
03 0 ---F-I (Ctl)
at$ T&Oe$nt bet"on OC and TOC values points towards lwmffioient of atie test astellal.
419141 an values detweimm oftsr somwoo fittlotsea.
soluoility
SPtJ-&,Aol-E,'PAr,F, fO P. 13L4@tJK DA-RA
0.140 It.1
ilage io
E
,je 12
"Ready Hiodegrad ability: Modified OECD Screening Test"
41
3
C: Eva:tjatlon
IDOC - concentrotionsi lslrtus lblanks
II
1 I 1 I
of raw data.
irlaski
Ino.
1
I
I
ol
II
1
,"It 03t
el
12
I
P:
0 21
L
12
-
lseen 1 01 02
I
ID $
2
for day x
03t -3 j
2-C)
IS 5,)Cremovalafter x day6 141 211 271 28 I1
P7.q I
.,P,it'd
"0 lq3.1 @-v.411 1Iit31,11
L)115-l7i4-''7179'r17 i
(AL-TS PIPF'AR -T,, s t+a L,@ r,4 L E
It 0 DOC
A W4
"A-T
U A L t4
ONE
',f7
30'1 E g e
"Ready Uiodegradability:
Nddified OECD Screening Test-'
I Page 11
S. A N N & X
IWLE F(HIM SHEET FOR IHE MODIFIEU QECD SCNEENIN G TELT
Exp. no.
i)oteor st-artor test: Io - ,)-I- X'4-
4wn4-* Standard ctetorl;li
Thearpli@t!
L;onc.:
inoculum: <,cco tjo#AAY r 4.41rggn eolf&Y%iSr:-DC - 6,2
.4n- I...-"tAI-AL.A@
ORA 4@so
ipgicfj@
At
I TOC* I DW*t I
1f*(*SGCk solution or the test material 1000 mg/l, dilution
1_ .../IDOO a] of nuirient sol-il-t-i-O.ftyA
Bt Carbon datere
3
1 -1
Te3-r
FI&Sicl Antlys4o
Culture sodium Ino. I
bUneral nutrl*nti
tion flift I I
Is,:I.u,motor- 9"
and w"us
noo
1
I
I
62
&1
4b (Ct)
f -bi
Coo
Th Or.1 UUL; - concentrations orter x days
llco:c. 1
40/1
so/I 10 (C())Imb7laal4lo*21lso271 28 1
021
-I 1
i
S,
1
I 1,4,101
A I-
0
J3.
1
iilit
:6-2 iil.3 1'q, -6 '16,21,1--0-S;:-73-
1
1
1
1
"P
I
7,9 i'qL, -q.Z
bl b2
1
142 a
I(Ct)
Rtneral nutrienti
I
solution without lianki
test noterLit-I
I
but in
lif
lnsev=vo
I
el
al 22
-
Cbl)
"Sutton withou testaftemym win saw-=
Blank
3.1, ;Ilsl
I
0 otooore"Wnt
between OOC and TOC Value$ OGL"tg
or %ft test "Sells&.
towards
sr4urrisiont
ALI M vidwe desenta" after embeens filtration.
solubility
@j;a0 A "-r-
age '121
E
12
"Ready.Siodograda bility: Modified OECD Screening Test"
C: leve:otion of -raw date:
[Flooki lno.
1
IOM - conoontrationel
lainus
I
Olt 101
IX DX removol arter x asy-6
1 71 141 211 271 28 1
Lao
01
12 I
L
62
,seen 1
01 02
I
for
2 doy
x
ino I
N3 J
iV7, I
1 1
I
I
I
I
177 19.5-1 p 1I I
de
Page 13
T-T 11
)0% @0%
iff ui
CYX
,C)% cr_ uj
cyx0%
0%
0
Appendix 2
3M Environmental Laboratory OECD Modified Screening Test with DOC Analysis Analyst: Wade A. Scheil Date of Start of Test: /o-.27-92Lab Request No.: I?zlf3
Test
Material:
Sc>j>t(AP4
fW-Pe-OA-rE
1
14
21
NUMBER OF DAYS INCUBATED
2@ 18
Page 14
44- 1 1 1
lwx
8m
C
7CYX
60%--g
50X CD
4(r/.
3CYX-
2aX
3M Environmental Laboratory OECD Modified Screening Test with DOC Analysis Analyst: Wede A. Schell Date of Start of Test: 10- 27- T 2Lab Request No.:
Test Moteris I FC-- 10 3 (A M-rL--f*t
7:
. ...............
14
2
NUMBER OF DAYS INCUBATED
Page 15
-4-4 1 1 1 f
IIf1
3M Environmental Laboratory
OECD Modif led Screening Test
Analyst: Wode A. Schell Date of Start of Test: Lab Request Ito.:
with
DOC Analysis
Test Material:-- C--(o
AP-ru)E-KP)
<
70% LLI I:c
60%-
5 (Y/.
40%-
LU gn
30%-
2 fPk ===Z
10%.
21 NUMBER OF DAYS INCUBATED
Form 6747-1 1-0
TECHNICAL REPORT SUMMARY
TO: TECHNICAL COMMUNICATIONS
CENTER - 201-2C-12
(Important- Ifreportisprintedon bothsidesofpaper,send two copiesto TCC.) Guidelineson reverseside.
Division
Dept. Number
P.nvi rc)nmpnt-al
Project
,is0,@.Fn a
Mncii f ipd nFrD To
T.ahorat-nrV
( F.P. F. PC) St- - Paul , Minnesota
qr rppn inq Tt-.-,tn-n FC- 20 -4, FC- 20 3A, a nd
' 5 Proje@,112,1.r
9.-7g0010100
ReporNtumber
FC-600
0 C)
Period Covered or Date
A@t@o,t@)' -P
Tc)Xirr)lr)q@i,
'IM C.PrmanV -
.,ence
Fnl.7irnnmpntal
T.AhnratorV
- 91-2W-05
7
Employ. Z3l@.@t4ert,@ 47816
No. ofPagesIncludinCgoversheat
Nnnp - qpp Pnvironmpntal
T.ah Reclilest #9@ll
1 ?--
SECURITY 100 OpenReport&Summary E3CloseRdeport-OpenSum,mary3MRCEHGEIMSITCRAYLb,0!: cCahleRcekgbiosxtiFrfnoyerwmc6h0e9m2itcoraaelrpseorraetlplonretwesUdus.besCthaenmcie-s.
KEYWORDS: LabCode
OtherKeywords
CURRENT OBJECTIVE:
To test the repeatability of the modified Test in measuring the biodegradability of products.
OECD Screening Light Water
REPORT ABSTRACT: ThisabstraicntformatiiosndistribubtyedtheTechnicCaolmmunicationCsentertoaler3tM'ertso Company R&D.
This study again used the modified OECD Screening Test to evaluate the biodegradability of Antwerp Light Water products. The products studied in this set of tests were FC-203, FC-203 NFP (equivalent to FC-203A), and FC-600. Also tested was U.S. FC-203 Lot 3072. One of these products, FC-203 NFP, was also included in the previous set of tests done in 1980. The results of this testing were consistent with previous OECD Screening Test studies on Light Water products. The results indicate that all of the tested products are readily biodegradable.
cc: R.L.Bohon-21-2W-05 D.R.Ricker-235-lB-10 D.W.Kent-236-2A-04
nfor atio . ison :nitialms: Irri
IPT
MODIFIED OECD SCREENING TEST ON FC-203, FC-203A, AND FC-600
INTRODUCTION
This study was undertaken to demonstrate the biodegradability Light Water (L/W) products, FC-600 and FC-203, using th internationally recognzied Modified OECD Screening Test Ti)
testing was requested by 3M Germany because of inconsistency
results of past biodegradation tests done on these products.
of two
This in the
Modified OECD Screening Tests conducted in 1980 by the 3M Environme Laboratory showed that three L/W products were highly biodegradable ?@ll
The products tested were FC-203A (previously identified as FC-203 NFP),
FC-206, and FC-3017 (FC-206 freeze protected).
Greater than 90% of the
dissolved organic carbon (DOC) of these 3 products was removed during
the 1980 testing. See Table 1 for a summary of these results.
Table I
Results of 1980 Testing on Light Water Products
Product
7
FC-203 NFP 1 13
FC-206
23
FC-3017 2 37
3
Hydroquinone
89
% Degradation at Day:
14
21
27
28
85
93
91
93
90
94
93
92
94
96
96
95
92
97
94
93
Footnotes:
1 FC-203 NFP is nonfreeze protected FC-203 and is equivalent to FC-203A.
2 3 FC-3017 is freeze protected FC-206.
Hydroquinone was the reference product.
These 1980 results contradict those of H. Hellmann a?q)D. Muller (3) who
used a similar test method, the TOC Degradation Test
. Hellmann's
TOC (total organic carbon) test results, however, are an exception from
normally obtained results. His finding of 8% TOC removal for FC-3017
and 6% TOC removal contradict his own
(BOD) results were
for FC-206 in the 21-day long TOC Degradation Test BOD 5 /COD data. His 5-day biochemical oxygen demand 50% and 40% of the chemical oxygen demand (COD) of
FC-3017 and FC-206, respectively.
This is a significant level of
degradation for a 5-day BOD test. These opposite results within his
own paper clearly are an inexplicable discrepancy.
Hellmann's TOC Degradation Test results are also inconsistent with
BOD /COD measurements made by the 3M Environmental
Laboratory and by
othip independent laboratories on 3M AFFF products.
Such results
typically show BOD
values to range between 60% and 90% of the COD.
For example, a coli2ction of such data on 3 U.S. military specification
AFFF products manufactured by 3M is shown in Table 2.
OECD Page July
Screening 2 9, 1894
Table 2
BOD, Carbonaceous BOD, and COD Data on Mil-Spec AFFF Product
BOD
C-BOD
COD
BOD
C-BOD
Lab (mg/@8) (mg/k@? (mg/kg) co@o COD 20
FC-203 C Lot 501
3M
580,000
600,000
730,000
.79
.81
740,000
Pace
800,000*
730,000*
810,000
730,000
Serco
440,000
440,000
737,000
.60
.60
Capsule
570,000
620,000
950,000
.6
.65
Galbraith
616,000
671,000
776,450
.79
.86
inoculum #1
Galbraith
670,000
641,000
776,450
.86
.82
inoculum #2
Average S. D.
575,000
594,000
782,000
.73
.75
85,000
90,000
80,000
.12
.12
Calculated BOD's from different dilutions were very inconsistent.
3M
Pace Serco Capsule Galbraith
inoculum #1 Galbraith
inoculum #2
290,000
350,000 240,000 260,000 416,500
395,500
FC-206C Lot 502
290,000
370,000 260,000 320,000 411,000
380,000 360,000 450,000 370,000 410,000 407,250
374,000
407,250
0.78
0.78 0.65 0.63 1.02
.97
0.78
0.82 0.70 0.78 1.01
.92
Average S. D.
325,000
338,000
396,000
.81
.83
73,000
57,000
33,000
.16
.11
3M
Pace Serco Capsule
Average S. D.
FC-780B Lot 501
240,000
230,000
320,000
.74
.71
330,000
250,000
250,000
350,000
.71
.71
210,000
220,000
287,000
.73
.77
240,000
230,000
360,000
.67
.64
235,000
232,000
329,000
.71
.71
17,000
13,000
28,000
.03
.05
OECD Page July
Screening 3 9, 1984
METHODS AND MATERIALS
1. Procedure
Testing was performed in accordance ,with t@?)OECD Guidelines for testing of chemicals adopted May 12 1981.
2. Chemicals
The reference materials used were laboratory grade sodium benzoate, (C H NaO ) F.W. = 144.11 and linear alkylbenzene sulfonate (LAS). ThZ EAS 3olution used was a 5.68% active solution supplied by the U.S.Environmental Protection Agency as a reference material for biodegradation testing. The Light Water (L/W) test mateials used were U.S. FC-203 Lot 3072 provided in 1983 by the Commercial Chemicals Division, FC-203 and FC-600 samples provided by E.T.S.L. Antwerp in 9/82 and FC-203 NFP provided by E.T.S.L. in 1980. Antwerp provided no lot numbers with their samples. FC-203 NFP (nonfreeze protected) is equivalent to FC-203A.
Prior to testing, the L/W and reference materials were dissolved it@l
the OECD nutrient solution and brought to the following initial
DOC concentrations:
sodium benzoate 20 mg/l, LAS approximately 15
mg/l, and L/W products approximately 40 mg/l. The L/W TOC was
higher than that used in previous testing (20 mg/1) because our
experience has shown that L/W at 40 mg/l is not toxic. Also higher
concentrations improve the accuracy of the TOC analysis.
For this study, nutrient solutions were prepared using both vitamin sources allowed by the OECD Screening Test, yeast extract and synthetic vitamin solution. This was done to determine if the vitamin source affected the extent of L/W degradation.
INOCULUM
The inoculum was a 50/50 mixture of soil extract and secondary effluent prepared in accordance with OECD procedures. The soil, which was extracted, was a mixture of fresh, sandy loam garden soils obtained from Ramsey and Washington Counties in Minnesota. The secondary effluent sample was the supernatant of an activated sludge mixed liquor sample taken from an aeration basin at the St. Paul Metro Wastewater Treatment Plant. The combined inoculum was passed through Whatman 54 filter paper prior to usage.
INSTRUMENT
The organic carbon analyzer used was a Dorhman DC-52A. limit is approximately 2 mg of carbon per liter.
Its sensitivity
OECD Page July
Screening 4 9, 1984
SAMPLE HANDLING AND STORAGE
The sample preservation method used was that
escribed by the
manufacturer of the organic carbon analzyer. (F@ The method involves
adding 1 drop of concentrated HC1 per 10 ml of filtered sample. This
brings the samples to less than pH 2. The samples were stored under
refrigeration in vials with aluminum foil lined caps. our experience
is that this storage method can preserve L/W containing samples for
several months without affecting the DOC. All DOC analyses on samples
from this study were done within one week of its completion.
RESULTS AND DISCUSSION
Table 3 summarizes the results of this study. This table shows that sodium benzoate, the reference compound, was nearly completely degraded (95%) within 7 days. Every replicate of all of the L/W products showed greater than 80% TOC removal within the 28-day test period. Seven of the ten test flasks containing the various L/W products showed greater than 90% TOC removal. The average DOC removal for all four L/W product was greater than 90%.
The results of this testing are shown graphically in Figures 1 and 2.
These results are averaged, and because of this, do not show the actual
pattern of degradation in the individual cultures. Figure 3 is an
example graph of 2 cultures degrading the same product, FC-203 NFP. it
shows that once degradation of this product began that it was very
rapid, but that the lag prior to the onset of degradation was variable.
The reason for this variability between the duplicate cultures was not
known nor was it expected.
It may have been due to the fact that the
cultures received different levels of viable microorganisms capable of
degrading the major components of the Light Water products.
Thus, the
population of bacteria with these capabilities had to build up in the
cultures prior to the onset of rapid (exponential) degradation.
Review of the data in Table 3 indicates that results of replicate
testing of the other L/W products also varied considerably at days 7,
14, and 21. Again, this variation appears to be due primarily to the
length of the lag phase prior to the onset of biodegradation.
However,
due to the small number of samples taken, one frequently could not tell
how long biodegradation of individual L/W containing cultures took
following the initial lag.
OECD Page July
Screening 5 9, 1984
Biodegradation
Table 3 of LIGHT WATER Products
and Refernce
Materials
Product/Vitamin
Source
Sodium Benzoate/Yeast-I Sodium Benzoate/Yeast-
?2) Sodium Benzoate/Vit.-I Sodium Benzoate/Vit.-2
Mean
(3)
FC-203
/Yeast-1
FC-203/Yeast-2
FC-203/Vit.-l
FC-203/Vit.-2
Mean
U.S. FC-203/Yeast-I U.S. FC-203/Yeast-2
Mean
(5)
FC-203A
/Yeast-1
FC-203A/Yeast-2
Mean
FC-600 3 /Yeast-1 FC-600/Yeast-2
Mean
LAS/Yeast-I LAS/Yeast-2
Mean
7
98.8 99.6 94.4 88.6 95
11.7 29.5 29.4 24.8
26.9 64.3
12.6 13.2
6.6 7.7
22.8 5.9
% DOC Removal After X Days
14
17
21
27
28
30.5 29.1 32.6 88.6
25.1 90.8
8.5 89.1
75.5 10.5
7.8 8.8
--(4)
28.4 27.0 27.7 90.2
89.8 91.0 80.5 95.6
79.2 90.7
95.5 96.0
11.0 85.1
86.4 92.5
89.3
--
76.3
87.0
25.1 20.4
30 --tg)
49.1 29.7
95.3 92.1 83.6 95.2 92
96.5 97.5 97
87.2 96.0 92
94.2 88.8' 91
52.1 33.4 43
Footnotes:
(1) (2) (3) (4) (5) (6)
Used yeast extract Used OECD synthetic From Antwerp 1982. 17-day samples were From Antwerp 1980. Sample contaminated,
as vitamin source. vitamin solution as
only taken originally
not used.
for LAS. labelled
vitamin FC-203
source. NFP.
READY 100
l'igure i
BIODEGRADABILITY: Mod@fLed Screen'tng Te OECD 301E -- Ado ted 12 Ma@ 81
EnvLronmentaL Lob @equest No. 9611
THIS SERIES WAS RUN USING
90
'STANDARD' NUTRIENT SOLU TION
CONTAINING YEAST EXTRRCT.
............................................................................................................
n
C3 0
0Z so
cr_ C3 40
cr_C-9 LLJ C3 30
m
................................................................................../........................ ",Ppo
olp"
......
cr
1:7
......./.-.-.-.*...............................................-........................ /* ....
Legend
A uisFznx
20 .....
..................................................L....... ....x..So.Om.Im.)o.IoLmIN
0 FO-203
0 FC-203. 10
[1 FC-203 La
FC-6W,
OA
0
7
14
21
29
DAYS
READY 100
Figure 2
BIODEGRADABILITY: ModLfLed OECD 301E -- Ado ted 12
EnvLronmenta@ Lob @equest
Screen'tng T Ma@ 81 No. 9611
THIS SER IES w AS RUN USING
90
STANDARD NUTRIENT SOLUTION
WITH VITAMIN SOLUTION.
........................................................................................................ ............
C:) 70
C0-) 60 ..................................................................
..................................
:z so C:)
cr_
Ccr3_
4[) ............................................ ........................................................................... -/......
CD
00 30
-Z 20 ........................................................................................................
/000
Leger
A SODILIM
X FC-203
0
7
14
21
DAYS
Figure 3
READY BIODEGRADABILITYM:odLfLedScreen'unTgE OECD 301E -- Ado@ted 12 Ma@ 81
EnvLronmentaL Lob equest No. 9611
THIS SERIES WAS RUN USING 90 'STANDARD' NUTRIENT SOLUTION
CONTAINING YEAST EXTRACT.
80 ............................................................................................
C) 70
ci 0
60 ..........................................................................................................
C3
ZC3 5;0
C3 40 ....................................I................................................................................
CD ELI
0C) 30 m
20 ....................:./...............................................................................................
10
0
......
0
7
14
DAYS
Legend
1& PC-2m,
X PC-2M,
21
2
l'igure 4
READY BIODEGRADABILITY: ModLfLed Screen'tng OECD 301E -- Ado@ted 12 Ma@ 81
EnvLronmentaL Lob equest No. 9611
ioo THIS SERIES WAS RUN USING 'STANDARD* NUTRIENT SOLUTION CONTAINING YEAST EXTRACT.
so THE LAS REFERENCE WAS DILUTED WITH FRESH NUTRIENT SOLUTION
80 'ON TEST D19Y 29 AND RE-INOCULATED . ............................................. cr_
C:) 70
.............
..............
............. . ............
so 0
C3 cr_
40 ...........................................................................................
.........
C.9
C03 30
20 --- -------
10
0
0
7
------
Legend 1& utsIV m
Diu= utsm
14
21
28
35
42
DAYS
OECD Page
July
screening 9
9, 1984
The modified OECD Screening Test is intended for use on single chemical
substances.
L/W products, on the other hand, are aqueous solutions
containing a mixture of chemicals.
Pure chemicals, which have greater
than 70% loss of DOC within 28 days, are regarded by the OECD
guidelines as being readily biodegradable.
Also, this result has to be
reached within 10 days of the DOC removal first exceeding 10%. Only
one of the replicates of each of the four L/W products tested met this
second OECD requirement of 70% degradation within 10 days of first
reaching 10% degradation.
This requirement, however, is not
realistically applicable to L/W or other formulated products
(mixtures). The chemicals within mixtures will frequently have
differing susceptibilities to biodegradation.
Readily degradable
chemical components of such products may start to degrade immediately,
while the onset of degradation of other chemicals in these products may
be delayed. Thus, disregarding this second criteria, which is not
reasonable for mixtures of chemicals, the results show that the mixture
of chemical components in each of these products is readily
biodegradable.
Cultures tested with the synthetic vitamin solution a slightly lower level of DOC removed than cultures as the vitamin source. Future OECD screening tests yeast extract since the synthetic vitamin solution prepare and does not give improved degradation.
showed, on average, using yeast extract should thus use is more difficult to
LAS, which is a readily biodegradable and commonly used surfactant in
detergents, did not degrade fully under these test conditions.
This
occurred in spite of the fact that its concentration was only 15 mg/l
of DOC compared to the 40 mg/l of DOC used for the Light Water
products.
The reason for the slow rate of LAS biodegradation
appears
to be that LA Inhibited microbial degradation at the test
@6
concentration
. To check this hypothesis, at the end of the 28-day
test period, the remaining LAS containing test cultures were split and
half were diluted to twice their volume with fresh inoculated nutrient
media. At this point, the rate of degradation in the diluted cultures
increased substantially.
Seventy percent of the DOC remaining at the
time of dilution was removed within 15 days. Results of this work on
LAS are shown graphically in Figure 4. Another researcher, has
similarly reported a low level of biodegradation of LAS in the modified
OECD screening test. D. Liu found tha Tarlon A (dodecylbenzene sulfonate) had a half life of 39 days. t7
CONCLUSIONS
The present studies repeated the findings of previous OECD Screening
Tests on Light Water products done by the 3M Environmental Laboratory.
Both sets of tests showed that L/W products are "readily
biodegradable."
In all cases, the average DOC removal for L/W products
was greater than 90% after 28 days. L/W products were much more
degradable than the very commonly used and "readily biodegradable"
surfactant, LAS.
OECD Page July
Screening 10 9, 1984
REFERENCES
(1) organization for Economic Cooperation For Testing of Chemicals, Section 301 Modified OECD Screening Test, May 12,
and Development, Guidelines E, Ready Biodegradability: 1981.
(2) E. A. Reiner, Biodegradation of "LIGHT WATER" 6/80, 3M Technical Report No. 40, Dept. 0535, 6/30/80.
Products in OECD Test Project 9970012600,
(3) Dr. H. Hellmann and D. Muller, "Environmental Impact of Fire
Extinguishing Foam Compounds (Umweltgefahrdung durch
Feuerlosch-Schaummittell)."
The study was carried out by the
l@est German Institute of Hydrology (Bundesanstalt fur
gewasserkunde), April 18, 1979.
(4) D. Muller and T. Tittizer, "The TOC Degradation Test - A Process to Test Organic Materials for Complete Biodegradation (Der TOC Abbautest - ein Verfahren zur Prufung von organbischen Substan'_zen ii-ufVollstandigen Biologischen Abbau)." Developed at the Bundesanstalt for Gewasserkunde, Koblenz, Z. F. Waser-und Abwasser-Forschung (1979).
(5) Dohrman DC-52A Operating Manual, 4th Ed., 1978.
(6) R. D. Swisher, Surfactant Biodegradation, Marcel Dekker, Inc., 1970.
pages 16-17 and 147,
(7) D. Liu, Study on Biodegradation of Aniline and Marlon A, Biodeterioration 5, Edited by T. A. Oxley and S. Barrry, 1983.
L/W TOC ofFC- 600
%in Prod Components
EmpericalFormula MW
2 Sultonefoonier
Cl 6 H23 F13 32 06 N2
1 Filrmr(FC-95) C8 Fl7SO3 K
1 Na octylsulfate
CS H 17 04 3 Ne
1 No decylsulfate
Cl 0 H21 04S No
0.1 DowicideA
C 12 H 17 05 Ne
0.05 Benzotriazol
C6 H5 N3
0.8 KelcoKeltrol
assurm C6 H 10 04
0.8 StanleyH-277 Starch assume C6 H 10 04
12 ButylCarbitol
C8 HI 8 03
81.25 DI Water
H2 0
MWof C TOC
650 192 0.0059
522 128 0.0025
232
96 0.0041
260 120 0-0046
264 144 0.0005
119
72 0.0003
146
72 0.0039
146
72 0.0039
162
96 0.0711
18
0
0
Product TOC=
0.097 g/g
Page I