Document Bw22EVa92R9oyqNOmgzxOrdo
BIODEGRADATION (METHYLENE BLUE ACTIVE SUBSTANCE)
TEST SUBSTANCE
Identity:Perfluorooctanesulfonylamido(ethyl)acetmaatye;alsobe referredtoas PFOSAA, FC-128 oras the major component of FC-1 27, FC-129, FC-1 09, FC-1 09-X or Rl 904. (Glycine,Nethyl-N-[(heptadecafluorooctyl)sulfopnoytla]s-s,ium salt,CAS 2991-51-7)
Remarks: The testsample isFC-129 referretdo by thetestlaboratory as sample G1208-1 and replicataenalysisas sample G1208-4. Current informationindicatesitisa mixtureof42% testsubstance,32% water, 14% 2-butoxyethanol4,% ethanol,and 8% C4-C7 fluoroalkyclarboxylate compounds. Test materialwas from 3M productionlot564.
The followingsummary isabbreviated because the testsample isa mixture of the testsubstance in a waterlorganicsolvent solution. Data does not accuratelyrelatebiodegradation of the testsample with thatof the testsubstance.
METHOD:
Method: EPA Method 425.1 Type: Methylene Blue ActiveSubstance GLP: No Year completed: 1989
RESULTS
G1208-1: 2200 mg/kg G 1208-4: 2800 mg/kg (duplicatoef G1208-1) DuplicateEPA LAS Reference samples:60,000 mg/kg
60,000 mg/kg
CONCLUSIONS
This testingindicatedthatthe testsample exhibitedminimalactivitiynthis MBAS study.
Submifter: 3M Company, EnvironmentalLaboratory,P.O. Box 33331, St.Paul,Minnesota,55133
DATA QUALITY
ReliabilitKyl:imiscrhankin2g. Thisstudylacksinformatioonnthe methodology and testingparameters. Test substance puritywithinthe test sample was not sufficientclhyaracterized.
REFERENCES
This studywas conducted at Pace AnalyticaolfMinneapolis,Minnesota at the requestofthe 3M Company.
OTHER
Last changed: 5/17/00
ENVIRONMENTAL LABORATORY FINAL REPORT
1
REVISED
LAB REQUEST NO. G1208
REOUESTOR NAME: EA REINER DEPARTMENT: 0535 PROJECT NO: 9970010100 DATE RECEIVED: 02/03/1989 DESC: MBAS OF FC-129, TRITON H66
CONTRACT LAB: PACE
CONTRACT LAB COST: 162
3M E-L HOURS:
0
EXP COMP DATE: 02/17/1989
DATE COMPLETED: 02/15/1989
SAMPLES SHOULD BE DELIVERED IN MY NAME TO THE LAB. RUN A MEASUREMENT ON THE
STANDARD LAS SOLUTION FOR COMPARISON. DO ALL EXTRACTIONS AND BACK WASH CALLED FOR IN PROCEDURE. FC-129 IS 50% SOLIDS. ITS MW IS 623. THE MW OF THE LAS
STANDARD IS PROBABLE ABOUT 325. TEST FC-129 AT A MOLAR CONCENTRATION THAT OF LAS.
EQUAL TO
G1208-3 IS AN EPA LAS REFERENCE MATERIAL: LOT #1138, AVE. H.W. 318, ACTIVE LAS 6.00 %, PREPARED BY EMSL CINCINNATI US EPA IN COOPERATION WITH SOAP AND DETERGENT ASSOCIATION, DATE 985.
Revised report shows correction in project description above.
--------------------------------------------------------------------------------
SAMPLE DATE
CODE
DESCRIPTION
RESULT
MIN DET LIMIT
--------------------------------------------------------------------------------
1
FC-129
LOT 564
*SURFACTANTS - MBAS
2200 MG/KG
5
*INORGANIC TESTS REPORT
SEE ATTACHED REPORT
2
TRITON H66
RH-RM 6-1536
*SURFACTANTS
MBAS
1000 MG/KG
5
3
LAS STD.
EPA LOT 1138
*SURFACTANTS
MBAS
60000 MG/KG
5
4
DUPLICATE #1
*SURFACTANTS - MBAS
2800 MG/KG
5
5
DUPLICATE #2 ------------
*SURFACTANTS - MBAS
1200 MG/KG
5
6
DUPLICATE #3
*SURFACTANTS - MBAS
60000 MG/KG
5
* = CONTRACT LAB
SUBMITTED BY: k,
-DATED:-,.2-.;L
REPORT OF LABORATORY
pt[alblogr=.atoriensc,.
ANALYSIS
February 10, 1989
Offices: Minnea;)olisM.inne--ota Tampa, Florida CoraMile,Iowa Novato,California
&/Zo?
Mr. Wade Scheil 3M Environmental Laboratory 935 Bush Avenue Bldg. 2-3E St. Paul, MN 551-33
Dear Mr. Scheil:
Enclosed is the report of laboratory analyses for samples received 02/03/89. If you have any questions concerning.this report, please feel free to contact Tom Halverson or me. Sincerely.
RogenrC. Splinter, Ph.D. Director, Laboratory Services
Enclosures
1710 Douglas Drive North 0 Minneapolis, MN 55422 Phone (612)544-5543
an ecual codortunitv eme)tt)ver
REPORT
mbbofiotroie5l,rc.
3M EnvironmentalLaboratory 935 Bush Avenue Bldg. 2-3E St. Paul, MN 55133
OF LABORATORY ANALYSIS
February 10, 1989 PACE Project Number:
Offices: Minneapolis,.Minnftota Tampa.Florida CoralviIlolwea. NovatoC.alifomia
890203509
Attn: Mr. Hade Scheil
G1208
Date Sample(s) Collected: By Client Date Sample(s) Received: 02/03/89
PACE Sample Number: Parameter
I14ORGANIC ANALYSIS INDIVIDT)AL PARAMETERS Surfactants(1)
Units mg/kg
032110 MDL G1208-1
032120 G1208-2
032130 G1208-3
5
2200
1000
60000
MDL
Method Detection Limit
1710 Douglas DriveNorth0 Minneapolis,MN 55422 C3Phone (612)544-5543
REPORT
laboratories,,nc.
Mr. Hade Scheil Page 2
OF LABORATORY ANALYSIS
Offices:
MinneapolisM.innesota Tampa, Florida CoralvillIeo,wa Novato,Califomia
February 10, 1989 PACE Project Number: 890203509
PACE Sample Number: Parameter
INORGANIC ANALYSU INDIVIDUAL PARAMETERS Surfactants(1)
Units mg/kg
032140 MDL G1208-4
5
2800
MDL (1)
Method Detection Limit Analysis performed by EPA Method 425.1.
032150 G1208-5
1200
032160 G1209-6
60000
The data contained in this report were obtained using EPA or other approved methodologies. All analyses were performed by me or under my direct supervision.
Thomas L. Halverson Inorganic Chemistry Manager
1710DouglasDriveNorth0 MinneapolisM,N 554220 Phone (612)544-S543 an equal oDDortunity eMD10ver
AKALYSIS: MBAS
DATE ANALYZED: ANALYZED BY: TIME:. DATA REVIEW ED BY: ENTERED BY:
211-0137 72:@@
SMPLE
S)K
ANALYSIS 1--krguL-ys UNITS COMMENTS
@51cl I /Co
Z cT-7qI
32)1 3Z)2
1Z200 1/1000
Iptfll1i
lrr6lkIf
3 Z13 160io0ol
,321LI 2elpoo
ICO ml
.',Ave Z8
4P-,l 1 3100
,?ZI5 ze6>
.32/6 &0/0-00
FOR CLP USE ONLY?
CLIENT NAME: PROJECT-NUMBER: PROJECT NAME: FILE DATE -RECEIVED:. DATE COLLECTED.:
ml Sample
/00
IDO
1
ABS ug LAS
0
.2155 160 4.005 4
zz_ O.C)Z
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oozsr iz
BIODEGRADATION
TEST SUBSTANCE
Identity:Perfluorooctanesulfonylamido(ethyl)acetmaatye;alsobe referredto as PFOSAA, FC-1 28 or as the major component of FC-1 27, FC-1 29, FC-1 09, FC-1 09-X or Rl 904. (Glycine,Nethyl-N-[(heptadecafluorooctyl)sulfopnoytla]s-s,ium salt,CAS 2991-51-7)
Remarks: The testsample isFC-129. The study-definecdomposition is50% Potassium fluoroalkylcarboxylate,18% butylcarbitol2,8% water, and 4% ethanol.This isa minor contradictiotno theformulationavailable from proprietar3yM databases indicatinigtisa mixtureof42% test substance,32% water,14% 2-butoxyethanol4,% ethanol,and 8% C4-C7 fluoroalkyclarboxylatecompounds. Test materialwas from 3M Deutschland productionbatch 2304.
The following summary isabbreviated because the testsample isa mixture of the testsubstance in a waterlorgank solvent solution. Data does not accurately relatebiodegradation of the testsample with that of the testsubstance.
METHOD:
Method: OECD 301E
Type: Aerobic
GLP: No Year completed: 1984
Contact time: 28 days lnoculum: Secondary
Effluenotf a domestic sewage
plant
RESULTS
Mean DOC removal after28 days: 90%
Remarks: Organic carbon contentofthe testmaterialwas determined tobe 13.5 mg/l 00 mg sample by a carbon analyzer.
CONCLUSIONS No reliablceonclusionscan be derivedfrom thisstudy.
Submifter: 3M Company, EnvironmentalLaboratory,P.O. Box 33331, St.Paul,Minnesota,55133
DATA QUALITY
Reliability:Klimischranking3. The digestiveprocedure ofthe instrumentused inthisstudy todetermineTOC isnotaggressiveenough to break the carbon-fluorinbeonds. The TOC isthereforeinaccurate.The calculatedTOC is22% compared tothe 13.5% obtainedby analysis. These resultsare expected tobe representativoefthe organicsolvents presentand notofthe Perfluorooctanesulfonyalm ido(ethyla)cetate.Lack characterizatioonftestsubstance and confirmationoftestconcentrations.
REFERENCES
This study was conducted at Research and ConsultingCompany AG, Ch4452 ltingen/Switzerlandatthe requestofthe 3M Company.
OTHER
Last changed: 5/17/00
ENVIRONMENTAL RISK ASSESSMENT OF FC-1 29
SUBJECT PRODUCT
Identity:FLUORAD Brand FluorochemicalSurfactantFC-129. Major component isPerfluorooctanesulfonylamido(ethyl)aceCtAaSte, # 2991-51-7
Remarks: The subjectproductisFC-129. Currentinformationindicates itisa mixtureof42% testsubstance,32% water,14% 2-butoxyethanol, 4% ethanol,and 8% C4-C7 fluoroalkyclarboxylatecompounds and is referredto inthe assessment as "...a solutionversionofFC-128."
CONCLUSIONS
This assessment isextremelysubjective.There isno data tosupport conclusionsthatitwill"enterthe environment invery low concentrations". Additionallyc,onclusionsare based on limitedhazard data.
Submifter: 3M Company, EnvironmentalLaboratory,P.O. Box 33331, St.Paul,Minnesota,55133
REFERENCES
The subjectassessment was conducted by E.A. Reiner ofthe 3M EnvironmentalLaboratory,Env. Assessment InquiryNumber 80681, Sept. 25, 1981.
OTHER
Last changed: 5/17/00
internCaolrrespondence cc: R. L. Bohon - 21-2W-05
Ta D. R. RICKER - COMMERCIAL
CHEMICALS DIV. - 236-IB-10
From: E. A. REINER - ENVIRONMENTAL
LABORATORY/EE
& PC - 21-2w-5
Subject: OECD BIODEGRADATION
TESTS ON Vft-A'-a9 AND FC-170C
Date: OCTOBER 24, 1984
We have received and FC-170C from
copies of the OECD Screening D. Reese of 3M Germany.
Tests on FC-129
The results og the FC-129 study incorrectly indicate that
ihis product is readily degradable.' This result does not
accurately represent the actual susceptibility of this
product to biodegradation
because the instrument used to
measure total organic carbon (TOC) uses a UV-persulfate diges-
tion method. The OECD Screening test does not require a
specific TOC method, but the digestive procedure of the
instrument used in this study is not strong enough to break
fluorine-carbon bonds. Therefore, these results, really only
show that the butyl CarbitolO and ethanol in this product are
biodegradable.
The results of the FC-170C study are more useful b@t still
inaccurate.
These results confirm our previous BO@ tests
that suggested partial degradation of the polyethylene glycol
portion of this molecule. Again, however, the results
obscure the fact that the perfluoro portion of the FC-170C
molecule is almost certainly not biodegraded.
The data in these reports confirm the inability of the UV-
persulfate digestion method used to degrade the perfluoro-
carbon portion of these products.
The measured TOC for
FC-170C was 24 mg C per 100 mg product while the calculated
TOC based product.
on formulation information is 38 mg C per 100 mg The measured TOC for FC-129 was 13.5%; its
calculated TOC is about .22%.
Because of the weak and inappropriate
TOC method used, we are
not going to add these results to our Product Environmental
Data Sheets. misinterpret
Customers and regulatory agencies would likely these results and think that these products are
more biodegradable
than they actually are.
EAR/mb
RC R E S E A R C N & C ONSULT
C ING
CO M P A N Y A 6
PROAECT
034244
f4
READY BIODEGRADABILITY: -MODIFIED OECD SCREENING TEST"
FOR FLUCRAD
REPORT
P.O. Box CH-4452 Itingen Switzerland Phone 061 98 52 52 Telex 966 L36 RCC CH
RCC PROJECT 034244 FLUORAD FC-129
CONTENTS
PREFACE
I
INTRODUCTION
2
MATERIALS AND METHODS
2.1 Chemicals
2.2 Experimental design
3
RESULTS
3.1 Degradation of test compound 3.2 Degrada@,tion of standard compound (aniline)
4
CONCLUSION
5
REFERENCE
6
TABLES AND FIGURES
pac3a 3 -4 4 4 4
5 5
6-11
ip
RCC PROJECT 034244
3
FLUORAD FC-129
PREFACE
Project
034244
Sponsor
3M Deutschland GmbH Postfach 643 D 4040 Neuss I
Study monitor
Reese
Testing facility Study director
R CC Research and Consulting Company AG CH-4452 Itingen/Switzerland
Dr. H. Ellgehausen'
Date: So te or@1984
hoh
Technical assistance
V. Wuethrich
Start of experiments
August 17, 1984
Date of completion
September 14, 1984
Archiving
Raw data, protocol, report, duplicate of report-.
RC C Research and Consulting Company AG CH-4452 Itingen/Switzerland
m6t- rKujLLI
UJ444414
4
FLUORAD FC-i29
-I- XN-RRODUCYXON
The objectives of the present test were to follow the biodegradability of FLUORAD FC-129 in a 28 days biodegradation test by following the DOC of the chemical in the incubation flasks by calorimetric methods.
PIA-RERMAL-S
A N D METHODS
2.1 Chemicals ------------The following chemicals were tested:
Standard compound:
Test compound: Composition-
Aniline Purity: 99.5 X
Fluorad FC-i29
Potassium fluoro alkyl
carboxylate
50'X
Butyl @@01
is 7.
Water
28 X
Ethanol
4X
Batch: 2304
Water solubility:
)2 g/l at 25 degrees centigrade.
The test chemical was Ijupplied by 3M Deutschland GmbH, an July 10, 1984.
2.2 Experimental design ------------------------
The study was run according to the OECD method (1).
REC PROJECT 034244
5
FLUORAD FC-129
3
RESUL-TS
3.1 Degradation of test compound ---------------------------------
The results Figure 1.
are presented
in SaMP12 Form Shg2t No I and
3.2 Degradation of standard compound (aniline) -----------------------------------------------
The results are presented
Figure
in SaMP12 Form She2t No 2 and
4
CONCL-USMON
The test compound, Fluorad FC-129, was degraded under the test conditions within 28 days to 90 X. The standard, aniline, wa:s degraded withih SWV2n days to 97 X. The compouncf is considered to b2 readily d2gradeabl2.
5
REFERENCE
OECD Guid2lin2 for tei@A'-ionfg Ch2MiCalS: 301 E: -Ready Biodegradabilityt Modified OECD Scr2ening
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-RCC PROJECT 034244
-FLUORAD FC!-129
7
Sample form sheet No. l.cont.
C Evaluation of raw data: -----------------------
------------------------------------------------------------------------
Flask No.
X DOC remova-I after x days
7 14 21 ','.'7 28
DOC-concentrations minus blanks
-----------------------------------------------
mlt-m3t
JL
DI
i - ------- - 1.00
87 84 89 89
mt -m3 I
I
-----------------------------------------------------
m2t-m3t
02
1 - ------- - 100
96 86 87 90
m2 -m3
-----------------------------------------------------
mean
D
Di + D2 -------
87 85 88 90
for day x -------------------I-----------------------------------------------------
Samples lost during analysis.
RCC PROJECT 034244
ANILINE
8
SAMPLE FORM SHEET FOR THE MODIFIED OECD SCREENING TEST: NO 2 ------------------------------------------------------------
Date of start of test: August 17, 1984
Test/Standard material: Aniline
Theoretical test conc.:
Inoculum: sec. effluent of a domestic (ARA-Birsig,Therwil, CH)
19.4 sewage
mg C/1 plant
Carbon analyser: Technicon Autoanalyser II,
Method-No. 451-76 W -----------------------------------------------------------------------
A: Organic carbon content of test material: 100 mg test material correspond to: 77.4 mg organic carbon
Stock solution of the test material (25 mg/1) ---------------------------------------------------------------------
Bt Carbon determinations:
----------------------------------------------------------------------
Flask Analyses Theor.
DOC
Culture medium No.
conc.
after x days mg/l
mg/.l 0 (CO) 7 14 21
27 28
----------------------------------------------------------------------
Mineral nutrient
solution with
I.
al
test material
and with
a2
inoculum
19.4 19.4
12.4 0 11.9 2.4
2.1 1.8
1.2 1.1
1.8 1.9 1.6 2.3
ai+a2 mJL ------ 19.4
2
1.2.2 1.2 2.0 1.2 1.7 2.1
bi --1-9-.-4---1-2-.-0---3-.-1---1-.-8--1-.-9----1-.-9--2-.-1-----
2
b2
19.4 10.9 2.7 1.6 1.4 1.8 2.1
bi+b2
m2n ----- -19.4 II.S 2.9 1.7 1.7 1.7 2.1
2 'g
:, I
-------------------------p--------------------------------------------
Mineral nutrient
cl
solution without Blank
1.3 1.13 1.2 1.4 1.6 1.9
test mal%.erial but with
C2
0.7 2.7 l..S 1.1. 2.4 2.1
----------------------------------------------
inoculum
cJL+c2
m3a ----- -
1.0 2.3 1.5 1.3 2.0 2.0
2 ---------------------------------------------------------------------
Value calculated. All DOC values determined after centrifugation.
rnujc6l 'ANILINE
Sample form sheet No. 2 cont.
Ct Evaluation of raw data: -----------------------
-------------------
-------------------------------------------
Flask.
I------------
No.
X DOC removail after
x days
7 14 2 J. 27 28
DOC-concentration5 minus
blanks
-----------------------------------------------------
i
Di
mit-m3t JL - ------- - loo 100 96 100 100 99
mi -m3 1
----------------------------------------------------- 1
2
D2
m2t-m3t - ------- - 100 94 98 96 100 99
M2 -m3
-----------------------------------------------------
mean
D
Di + D2
97 97 98 100 99
for day x ------------------------------------------------------------------------
Figure I
DOC-removal Test material: Fluorad FC 129
I
IL
Figure 2: DOC-removal Test material: Aniline
..............
.. ..... . .... .
.........
-
- ---------
Shosti
THOD of FC-129
1)50% FC SOLIDS: C8Fl7SO2N(C2HS)CH2COO-K+
11/91 NOTE: CARBON RATIOS ARE 04.CS.CO.C7,CS=2.5%.O 2)14% BUTYL CELLOSOLVE 3) 32% WATER 4)4% ETHANOL
53%.2%.42,.
FRACTK)N
coKm3aqENTS
42.00-% C8Fl7SO2N(C2HB)CH2COO-K+
2.00% C7Fl5SO2N(C2H5)CH2COO-K+
3.00% C6Fl3SO2N(C2HS)CH2COO-K+
0.50% C5FllSO2N(C2HS)CH2COO-K+
2.50% C4F9SO2N(C2HS)CH2COO-K+
14% C4
H20H
4%,CH3CH20H
32%[WATER
ioo.oo%lToTAL -A
PAN
MW CARBON % Carbon
-623
144
9.71%
573
--132
0.46%
523
120
0.69%
473
108
0.11%
423
96
0.57%
162
96
8.30%
4
24
2.09%
1
0.00%1
21.92%