Document 44YMjYaMVmYVvKjy6z6XMZwk1
AK.PA6 _ o7ll
BIODEGRADATION (301E)
TEST SUBSTANCE________________________________________________
Identity: A mixture containing perfluorooctanesulfonate, which may also be referred to as PFOS, FC-95, or as a component of FC-203. (1Octanesulfonic acid) (CAS # 2795-39-3).
Remarks: The 3M production lot number was not noted. The test sample is FC-203. Current information indicates it is a mixture of 1.34% PFOS, 35% diethylene glycol butyl ether, 37.85% water, 20% ethylene glycol, 2.66 % Sultone foamer, 3% sodium octyl sulfate, 0.1% sodium lauryl sulfate, and 0.05% tolyltriazole.
The following summary applies to a mixture with incompletely characterized concentrations of impurities. Data may not accurately reflect degradation potential of the fiuorochemicai component of the test sample.
M E T H O D _________________________________________________________
Method: Modified OECD Screening Test, OECD 301E, with DOC Analysis,
1981 version.
Test type: Ready Biodegradability
GLP: No
Year Completed: 1982
Analytical monitoring: Dissolved organic carbon (DOC)
Statistical methods: Results were determined by calculation of the % DOC
removal and graphic interpretation.
Test organism source: A 50:50 mix of soil extract and secondary effluent.
The secondary effluent was the supernatant from an activated sludge
aeration basin at the Metro Wastewater Treatment Plant, St. Paul, MN, while
the soil was from the City of White Bear Lake, Ramsey County, MN.
Test condition:
Dilution water: Deionized water
Mineral Nutrient Medium: Nutrient medium per OECD 301E method
(1981). Initial pH 7.0.
Reference and test solution preparation: The test material was
prepared by dissolving 153 mg in two liters of mineral nutrient medium.
This solution gives a final test concentration of 20 mg DOC/L. The
reference substance, sodium benzoate, was prepared by dissolving
30.3 mg in one liter of mineral nutrient medium. This solution gives a
final test concentration of 20 mg DOC/L.
Test vessels: Not given.
Incubation conditions: Constant dark conditions
Temperature:
23.5 - 24C
Agitation:
Continuously
000444
Number of concentrations: 1 plus sodium benzoate (reference substance) and blank, all in duplicate. Inoculum condition on test initiation: Not given . Element Basis: Decrease in dissolved organic carbon compared to the blanks. Test substance flask conditions: Not given.
RESULTS_________________________________________________________
Nominal concentrations: Blank control, sodium benzoate at -2 0 mg DOC/L and at -2 0 mg DOC/L plus HgCL2 (inhibited), test material at ~20 mg DOC/L and at -2 0 mg DOC/L plus HgCh, all in duplicate.
Element values: 27-day Degradation = 76.7% duplicate 1 and 81.3% duplicate 2. Mean value = 79%
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 FC-203 % degradation based on the mean DOC removal value was 79 after 27 days.
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, the 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 ____________________________________________________
The studies were conducted by the 3M Company, Environmental Laboratory, St. Paul, MN, Lab Request number 8483, 1982.
O T H E R ___________________________________________________________
Last changed: 6/27/00
00044
Internal Correspondence
cc: vD. L. Bacon/R. L. Bohon - 21-2W-05 i/R. Gritzky - 3M Neuss >/D. R. Ricker - 236-2B-01 i/J. A. Pignato - 236-2A-01
Co
Ao: K. F. SCHROEDER - 3M NEUSS, GERMANY
From: E. A. REINER - ENVIRONMENTAL LABORATORY/EE & PC - 21-2W-5
Subject: BIODEGRADATION TESTS
d
Date: APRIL 21, 1983
Envir. Assess. Inq. #82326 3M Neuss, Germany FC-203, FC-600
Attached is a copy of our report on the modified OECD screening tests on FC-600 and FC-203. While the results of this testing does not precisely repeat those which we obtained on FC-203 in 1980, they do confirm that FC-203 is readily biodegradable according to the test method criteria. The present results also show that FC-600 is readily biodegradable.
The reason that these results do not precisely match those of our previous testing is not known, but biodegradation test results are characteristically somewhat variable. This variability is often explained by one or more of the following three factors:
1. Differences in the bacterial species or strains present in the inocula of tests started at different times.
2. Variations in the formulation of a product from one lot to another.
3. The presence of inhibitory materials such as possibly toxic byproducts or inadvertent contaminants.
v* A
ft
000446
K. F. Schroeder Page 2 April 21, 1983
The percent biodegradation results given in the attached report are equally applicable to both the concentrated AFFF products, as sold, and the diluted products, as used. Dilution with pure water would have no effect. The reason for this is that testing is actually done on a very dilute portion of the concentrate (20 ppm as TOC). B o th H io c o n c e n t r a t e o r t h e 3 o r 6'l u s a g e l e v e l w o u ld be diluted to this same concentration for testing. The dilution factor is not considered when calculating the results.
I have reviewed the table of biodegradation data that you sent us. Some of the variability in results which you show is not unexpected. This is particularly the case with the 5-day BOD test results. Biodegradation of AFFF products is usually only partially completed within the first five days of a BOD test and .the percent of biodegradation that has been completed in this time period is highly dependent upon both the viability of the microbial inoculum and the fraction of the organisms in the inoculum which are capable of degrading the organic compounds.
Results of 20-day BOD tests are less variable because biodegradation is usually more nearly complete and proportion of organisms capable of degrading AFFF products has increased through growth. But, 20-day BOD tests are susceptible to another type of problem, "nitrification." In these longer tests, populations of bacteria can develop which can oxidize the ammonia in the BOD dilution water making it appear that the test material is more biodegradable than it actually is. In the Environmental Laboratory we are now taking precautions to avoid this problem by using "nitrification inhibitors," chemicals which inhibit ^the oxidiation of ammonia.
A point of confusion in your table of BOD data is the reporting of different BOD5 to COD ratios for both the undiluted and diluted AFFF products. This doesn't make sense because BOD and COD would decrease proportionally with dilution with the ratio remaining the same. These differences which you indicated were reported in Hellmann's work must therefore be due to variability between one BOD test run and another and not to dilution/
000447
K. F. Schroeder Page 3 April 21, 1983 We hope the attached OECD test results and this explanation of the biodegradation data in the table which you provided are helpful to you in dealing with potential customers concerned about biodegradation. If you or your customers have any further questions about biodegradation test results on 3M AFFF products, feel free to contact us. Wo'11 do our best in trying to get a satisfactory answer for you. and your customers. For our own benefit and at our expense, we are in the process of repeating the OECD screening tests on the FC-600 and FC-203 samples used in this testing. We are interested in seeing how repeatable our testing results are when the same samples are used in two separate tests. We will inform you of the results of this test.
EAR/mb Attachment: Report on the Biodegradation of FC-600 and
FC-203 by the OECD Screening Test
'V
000448
Form 6747-11-6
TECHNICAL REPORT SUMMARY
TO: TECHNICAL COMMUNICATIONS CENTER - 201-2C-12 (Im portant - I f report is printed on both sides o f paper, send two copies to TCC.) Guidelines on reverse side.
Division
3M Environmental Laboratory (EE & PC) St. Paul Minnesota
1'ioloci
3M Germany
Roport Title
OECD Biodegradation Testing on FC-600 and FC-203
To
K. F. Schrqeder, 3M Neuss, Germany
Au thor(s) , A
E. A.^ Reiner, Environmental Laboratory - 21-2W-05
Notebook Reference
None - See 3M Environmental Lab Request 8483
bept. Number
0535
Project Numbor
9972410100
Report Numbor
col
Period Covered or Dite
4/18/83
Employee Nurnber(s)
47816
No. of Pages Including Coversheet
15
ccr'i iD iT v w Open Report & Summary Q Closed Report--Open Summary 3M CH EM IC AL w, Check box if new chemicals are reported. Use Che:
b b u u m iv p
REGISTRY-- ~ xcal Registry Form 6092 to report all new substanci
KEYWORDS: Lab Code
Other Keywords
CURRENT OBJECTIVE:
1. To measure the biodegradability of two "Light Water" products using the internationally recognized Modified OECD Screening Test.
2. To compare results with those previously obtained using the same test method.
REPORT ABSTRACT: This abstract information is distributed by the Technical Communications Center to alert 3M'ers 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 AFFP products: FC-203 and FC-600. In 28 daysr the DOC levels of FC-600 degraded by 80% and 92% for an average of 86%"in two parallel tests. In 27 days the DOC of FC-203 degraded by 77% and 81% for an average of 79%. The FC-203 result differed from a similar test done in 1980 in which 93% DOC degradation occurred within 21 days. In the present studi parallel sterile controls proved that the DOC loss was not due to chemical or physical processes such as adsorption, volatilization, or precipitation of the organic compounds
Information Liaisi Initials:
000449
FC-600/FC-203 Page 2 April 18, 1983
Introduction The 3M Environmental Laboratory undertook this study of the biodegradability of "Light Water" products, FC-600 and FC-203, because of concern expressed by 3M Germany about inconsistencies in past biodegradation test results. Modified OECD Screening Tests conducted in 1980 by the 3M Environmental Laboratory showed that three "Light Water" products were highly biodegradable. FC-203A, FC-206, and FC-3017 (FC-206 F) all were shown to have 90% of their dissolved organic carbon removed in the OECD Screening Test. These results, however, contradict those of H. Hellmann and D. Muller^1) using a similar yet not identical test method, the TOC Degradation Test^). in their study FC-206 and FC-3017 were found to have total organic carbon reductions of only 6% and 8%, respectively, in 21 days. These low biodegradation results of Hellmann, however, were also contradicted by his own work. His BOD5/COD ratios for FC-3017 and FC-206 were 0.5 and 0.4, respectively. This showed that 50% and 40% of the theoretical oxygen demand was expressed within only 5 days. These levels of biodegradation are much 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 discrepancy in his work. Hellmann's TOC degradation results are also contradicted by BOD20/COD 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 example, a collection of such data on 3 U.S. military specification AFFF products made by 3M is shown in Table 1.
000450
Page 3
TABLE 1
UD, CARBONACEOUS BOD, AND COD DATA ON MIL--SPEC AFFF PRODUCT
BOD2Q
C-BOD
COD BOD?n C--BOD?n
Lab
Iissbfla l (mq/kq) (mg/kg)
COD
COD
' FC-203C Lot 501
3M
Pace
Serco Capsule Galbraith S & Vi Seed Galbraith Knoxville
500,000
'800,000*
1
440,000 ~ ` 570,000
616,000
670,000
-
600,000
730,000*
440,000 620,000 671,000
641,000
730,000 740,000 810,000 730,000 737,000 950,000 776,450
>
776,450
.79
.60 .6 .79 .86
.81
.60 .65 .86 .02
Average S, D.
575,000 594,000 782,000
85,000
90,000
80,000
.73 .12
.75 .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.
3M Pace Serco Capsule Galbraith S & W Seed Galbraith Knoxville
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.
3M Pace Serco Capsule
325,000 73,000
240,000 250,000 210,000 240,000
336,000 396,000
57,00
33,000
FC-780B L ot 501
230,000 250,000 220,000 230,000
320,000 330,000 350,000 287,000 360,000
Average
235,000 232,000 329,000
.8 P_________________ 17,000 13,000 28,000
.81 83 .16 .11
.74 .71 .71 .71 .73 .77 .67 .64 .71 .71 .03___________ .05
000451
FC-600/FC-203 Page 4 April 18, 1983
Methods and Materials
1. Procedure
Testing was performed in accordance with the OECD Guideline; lior testing of chemicals adopted May 12, 1981.
2. Chemicals
The reference material used was laboratory grade sodium benzoate (C7H5Na02 ) F.W. = 144.11. A 30.3 mg sample of this compound was diluted to 1.0 liters with the nutrient solution described by the method to yield a theoretical DOC of 20 mg/1. 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 "Light Water" products with DOC's of approximately 20 mg/1 (based on calculations from the formulation) were prepared by bringing both 527 mg of FC-600 and 153 mg of FC-203 to 2.0 liters with nutrient 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 Whatman 54 filter paper
prior to usage.
4. Sterile Controls
Replicate vessels containing 400 rag/1 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 TO( 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.
000452
FC-6Q0/FC-203 Pago 5 Aprii 18, 1983
Due to problems with the sensitivity of the TOC analyzer, only half of the samples were analyzed within a month after sampling. Following 4-5 months of storage, all of the samples were reanalyzed. Comparison of the TOC analyses done within 1 month with those done after 4-5 months of storage showed that in only one stored sample had the TOC changed significantly. This sample 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 a function of time. Table 2 shows that the sodium benzoate reference compound was nearly completely degraded within 14 days. Degradation of both FC-600 and FC-203 continued throughout the course of the 20-day test period without plateauing. At 28days the average TOC removal for FC-600 was 86% and at 27 days theaverage TOC removal for FC-203 was 79%. The test procedure recommends that chemicals giving a result greater than 70% loss of DOC (within 28 days) should be regarded as readily biodegradable. These 3M formulated AFFF products 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
Sodium Benzoate Sodium Benzoate Duplicate
2
94.4 92.3
% Degradation at Day: li 21 27 28
94.7 96.3
93.2 99.6
93.5
94.5
97.7 100.0
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 tophysical modes such as adsorption, volatilization, or precipitation. These samples were handled identically to the test vessels, except that they contained HgCl2 to prevent microbial growth. At the end of 28-day test period, these controls contained all of the initial DOC.
000453
FC-600/FC-203 Page 6 April 18, 1983
TABLE 3
Percent of Initial DOC in Sterile Controls at 28 days
Product
% DUC Remaining
b'C-203
98.1
FC-600
101.3
Conclusion
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 and FC-206 had average losses of DOC of 79% and 86%, respectively.
References
1. Dr. H. Hellmann and D. Muller, "Environmental Impact of Fire Extinguishing Foam Compounds (Umweltgefahrdung durch Feuerlosch-Schaummittell)." The study was carried out by the West German Institute of Hydrology (Bundesanstalt fur Gewsserkunde), April 18, 1979.
2. D. Muller and T. Tittizer, "The TOC Degradation Test - A Process
to Test Organic Materials for Complete. Biodegradation (Per TOC -
Abbautest - ein Verfahren zur Prfung von Organbischen Substanzen
auf Vollstndigen Biologischen Abbau)." Developed at the
Bundesanstalt for Gewsserkunde, Koblenz, Z. F. Waser^-und
v
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.
000454
Appendix 1
*. A N N E X
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2Appendix
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