Document dQb922mGDJKdKvk50ZzeKe2JG

/)R 6 _ 0-713 BIODEGRADATION (OECD 301 E) 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 numbers were Antwerp, Belgium 9/82 and US 3072. The test sample is FC-203 produced in Antwerp, Belgium. Current information indicates FC-203 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 o f impurities. Data may not accurately reflect degradation potential o f the fluorochemical component o f the test sample. M E T H O D ________________________________________________________ Method: Modified OECD Screening Test, OECD 301E, with DOC Analysis Test type: Ready Biodegradability GLP: No Year Completed: 1983 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. Fresh sandy loam agricultural soils from Ramsey and Washington Counties, MN. Secondary effluent, supernatant of activated sludge mixed liquor aeration basin, obtained from Metrow W astewater Treatment Plant, St. Paul, MN. Test condition: Dilution water: Deionized water Mineral Nutrient Medium: OECD medium using yeast extract, OECD medium using synthetic vitamin solution and OECD medium with reduced nitrogen content but using yeast extract. Reference and test solution preparation: Test and reference solutions were prepared for each of the three mineral nutrient mediums, except US 3072 only in OECD with yeast extract. Solutions were split into aliquots and put into Erlenmeyer flasks. Test materials prepared to give final test concentration of 40 mg DOC/L, reference standards at 20 mg DOC/L and 15 mg DOC/L for sodium benzoate and LAS respectively. Test vessels: One L Erlenmeyer flasks containing 500 mL test solution and capped with foam plugs. 0 0 0 4 ' 8 7 Incubation conditions: Continuous dark conditions Tem perature: 23.5 - 24C A gitation: Continuous Num ber o f concentrations: One plus references and blank, all in duplicate for each nutrient medium type. Inoculum condition on te st initiation: Not taken. Elem ent Basis: Decrease in dissolved organic carbon compared to blanks. Test substance flasks conditions: Not recorded. RESULTS_________________________________________________________ Nom inal concentrations: Test materials at ~40 mg DOC/L, sodium benzoate at ~20 mg DOC/L, LAS at ~15 mg DOC/L and Blank controls. Elem ent values: FC-203 Antwerp 9/82 28-Day Degradation = 94% mean DOC removal (yeast) 28-Day Degradation = 89% mean DOC removal (vitamin) 28-Day Degradation = 35% mean DOC removal (low nitrogen) FC-203 US 3072 28-Day Degradation = 97% mean DOC removal (yeast) Rem arks: 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. C O N C L U S IO N S ___________________________________________________ FC-203 Antwerp 9/82, mean degradation based on DOC removal ranged from 35% for the low nitrogen series to 94% for the yeast series, with 89% mean DOC removal for the vitamin series after 28 days. FC-203 US 3072, degradation based on DOC removal was 97% after 28 days. Subm itter: 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 purities were not properly characterized and the study lacks analytical confirmation of the amount of fluorochemical proportion in the solution. 000479 REFERENCES The studies were conducted by the 3M Company, Environmental Laboratory, 3M Lab Request number 9611, 1983. O T H E R __________________________________________________________ Last changed: 6/28/00 000480 Form6747-11-D TECHNICAL REPORT SUMMARY TO: TECHNICAL COMMUNICATIONS CENTER - 201-2C-12 (Important -- I f report is printed on both sides o f paper, send two copies to TCC.) Guidelines on reverse side. D ivision e pt. Number Rnvi rr>nm<an<-a1 L a b o r a t o r y fEE & PC)_St. P a u l Minnesota P roject 0 535 P roject N urnber ftWftffenatOnal _9 .97oni nino R eport Num ber Mndi.fi aH n w r n S r r p p n i n g Tas t on F f - 20 3,._F C - 2 0 3 A f_and F C - 6 0 0 ooZ T o P eriod Covered o r Date Aunth.or!*T)?AiagF>f T n v i r n 1 n g y f_R s n n a n y EmplZyee^'iumberf*) -E. A. Reiner - Envirxtnmental-- Laboratory - 21.-2W-Q5 N otebook Reference jjJ.SL16 N o . o f Pages In c lu d in g Coversheet -Mone - See Environmental Lab.Request #9.611 1*=L. SECURITY [jjOpen Report& Summary D Closed Report--Open Summary 3 M C H E M IC A L w Q Check box if new Chemicals are reported. Use ChemiR E G IS T R Y _ cal Registry Form 6 0 9 2 to rep o rtall newsubstances. KEYWORDS: Lab Code CURRENT OBJECTIVE: To test the repeatability of the modified 1III1I1-1,,I-M IIIM III Test in measuring the biodegradability of products. OECD Screening Light Water Other Keywords REPO RT A B S TR A C T: This abstract inform ation Is distributed by the Technical Communications Center to_alert 3M 'ers to 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-2Q3, FC-203 NFP (equivalent to FC-203A)r, .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 pro'ducts are readily biodegradable. > cc s R .L .Bohon-21- 2W-05 D.R.Ricker-23 5-1B-10 D.W.Kent-236- 2A-04 Informatiq, Initials: 3M CONFIDENTIAL 000481 X MODIFIED OECD SCREENING TEST ON FC-203, FC-203A, AND FC-600 INTRODUCTION This study was undertaken to demonstrate the biodegradability of two Light Water (L/W) products, FC-600 and FC-203, using the... internationally recognzied Modified OECD Screening Test' . This testing was requested by 3M Germany because of inconsistency in the results of past biodegradation tests done on these products. Modified OECD Screening Tests conducted in 1980 by the 3M Environmental Laboratory showed that three L/W products were highly biodegradable'2 . The products tested were FC-203A (previously identified as FC-203 N F P ) , 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 1 Results of 1980 Testing on Light Water Products Product % Degradation at Day; 7 14 21 27 28 FC-203 NFP1 13 85 . 93 91 93 FC-206 ,, 23 90 94 93 92 FC-3017^ 3 37 94 96 96 95 Hydroquinone-3 89 92 97 94 93 Footnotes: 1 FC-203 NFP is nonfreeze protected FC-203 and is equivalent to 2 FC-203A. 3 FC-3017 is freeze protected FC-206. Hydroquinone was the reference product. ^ These 1980 results contradict those of H. Hellmann and.D. Mu(ller (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 for FC-206 in the 21-day lonc^ TOC Degradation Test contradict his own BOD-/COD data. His 5-day biochemical oxygen demand (BOD) results were 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 BOD2Q/COD measurements made by the 3M Environmental Laboratory and by other independent laboratories on 3M AFFF products. Such results typically show BOD20 values to range between 60% and 90% of the CODFor example, a collection of such data on 3 U.S. military specification AFFF products manufactured by 3M is shown in Table 2. 000482 OECD Screening Page 2 July 9, 1894 2 Table 2 BOD, Carbonaceous BOD, and COD Data on Mil-Spec AFFF Product C - B O D on COD C--BOD,,n Lab (mg/iS) (mg/kgy (mg/kq) Boe COD^U FC-203 C Lot 501 3M Pace Serco Capsule Galbraith inoculum #1 Galbraith inoculum #2 - 580,000 800,000* 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 .82 Average S. D. 575,000 85,000 594,000 90,000 782,000 80,000 .73 .12 .75 .12 * Calculated BOD's from different dilutions were very inconsistent. FC-206C Lot 502 3M Pace Serco Capsule Galbraith inoculum #1 Galbraith inoculum #2 290,000 350,000 240,000 260,000 416,500 395,500 290,000 370,000 260,000 320,000 411,000 374,000 380,000 360,000 450,000 370,000 410,000 407,250 407,250 0.78 0.78 0.65 0.63 1.02 .97 0.78 0.82 0.70 L 0.78 f 1.01 .92 Average S. D. 3M Pace Serco Capsule Average S. D. 325,000 73,000 338,000 57,000 396,000 33,000 ' FC-780B Lot 501 240,000 250,000 210,000 240,000 230,000 250,000 220,000 230,000 320,000 330,000 350,000 287,000 360,000 235,000 17,000 232,000 13,000 329,000 28,000 .81 .16 .74 .71 .73 .67 .71 .03 .83 .11 .71 .71 .77 .64 .71 .05 * 000483 OECD Screening Page 3 July 9, 1984 H METHODS AND MATERIALS 1. Procedure Testing was performed in accordance with the.OECD Guidelines for testing of chemicals adopted May 12, 1981. ' 2. Chemicals The reference materials used were laboratory grade sodium benzoate, (C7H5Na02 ) F.W. = 144.11 and linear alkylbenzene sulfonate (LAS). The LAS Solution 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 in the OECD nutrient solution and brought to the following initial DOC concentrations: sodium benzoate 20 mg/1, LAS approximately 15 m g / 1 , and L/W products approximately 40 mg/1. 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/1 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 'V synthetic vitamin solution. This was done to determinevif 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. Its sensitivity limit is approximately 2 mg of carbon per liter. 0004S4 OECD Screening Page 4 July 9, 1984 s SAMPLE HANDLING AND STORAGE The sample preservation method used was that.prescribed by the manufacturer of the organic carbon analzyer. 1 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 v degrading the major components of the Light Water p r o d u c t s . $ 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 b e 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. 000485 OECD Screening Page 5 July 9, 1984 4 Table 3 Biodegradation of LIGHT WATER Products and Refernce Materials Product/Vitamin Source Sodium Benzoate/Yeast-1 Sodium Benzoate/Yeast-22 . Sodium Benzoate/Vit.-1v Sodium Benzoate/Vit.-2 Mean FC-203(3 V i east-1 FC-203/Yeast-2 FC-203/Vit.-l FC-203/Vit.-2 Mean U.S. FC-203/Yeast-l U.S. FC-203/Yeast-2 Mean F C - 2 0 3 A (5)/ Y e a s t - l FC-203A/Yeast-2 Mean FC-6003/Yeast-l FC-600/Yeast-2 Mean LAS/Yeast-1 LAS/Yeast-2 Mean __________ % DOC Removal After X Days 7 1 1 17 21 27 28 98.8 99.6 94.4 88.6 95 11.7 29.5 29.4 24.8 30.5 29.1 32.6 88.6 __(4 ) -- --- 28.4 27.0 27.7 90.2 89.8 91.0 80.5 95.6 95.3 92.1 83.6 95.2 92 26.9 64.3 25.1 90.8 ----* 79.2 90.7 95.5 96.0 96.5 97.5 97 12.6 13.2 8.5 89.1 ---- 6.6 75.5 7.7 10.5 11.0 85.1 86.4 9 2.5 __(6 ) 89.3 76.3 87.0 87.2 96.0 92 94.2 88.8 91 22.8 5.9 7.8 8.8 25.1 20.4 49.1* . 52.1 29.7 33.4 43 Footnotes: Used yeast extract as vitamin source. Used OECD synthetic vitamin solution as vitamin source. From Antwerp 1982. 17-day samples were only taken for LAS. From Antwerp 1980. Originally labelled FC-203 NFP. ' 1 Sample contaminated, not used. 000486 i'iyunj X BIODEGRADABILITY: Modified Screening Test OECD 30IE -- Adopted 12 Mag 81 Environmental Lab Request No. 9611 100 90 oa 70 60 50 iD 30- 20- 10- 0, figure )DY BIODEGRADABILITY: Modified Screening Test OECD 30IE -- Adopted 12 Mag 81 Environmental Lab Request No. 9611 100 THIS SERIES HRS RUN USING 90 STANDARD NUTRIENT SOLUTION WITH VITAMIN SOLUTION. / 80 / 70 / / 60 / 50 / / 40 / / 30 / 20 Legend 10 A SODIUM BENZOATE REFERENCE X PC-203, ANTWERP 9/82 0 1 -- -- r I 11 T I I "I r f r- r 7' 14 21 28 'D A Y S READY BIODEGRADABILITY: Modified Screening Test 'OECD 30IE -- Adopted 12 May 81 Environmental Lab Request No. 9611 i'lyuic * OECD Screening Page 9 July 9, 1984 fl 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 showed, on average, a slightly lower level of DOC removed than cultures using yeast extract as the vitamin source. Future OECD screening tests should thus use yeast extract since the synthetic vitamin solution is more difficult to prepare and does not give improved degradation. 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/1 of DOC compared to the 40 mg/1 of DOC used for the Light Water products. The reason for the slow rate of LAS biodegradation appears v to be that LAS,, inhibited microbial degradation at the test 'r concentration1 . 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 that_Marlon A (dodecylbenzene sulfonate) had a half life of 39 days. 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. 000491 OECD Screening Page 10 July 9, 1984 REFERENCES Organization for Economic Cooperation and Development, Guidelines For Testing of Chemicals, Section 301 E, Ready Biodegradabilitys Modified OECD Screening Test, May 12, 1981. (2) E. A. Reiner, Biodegradation of "LIGHT WATER" Products in OECD Test 6/80, 3M Technical Report No. 40, Dept. 0535, Project 9970012600, 6/30/80. (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 West 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 (Per TOC Abbautest - ein Verfahren zur Prfung von Organbischen Substanzen auf Vollstndigen Biologischen A b b a u )." Developed at the Bundesanstalt for Gewsserkunde, Koblenz, Z. F. Waser-und Abwasser-Forschung (1979). (5) Dohrman DC-52A Operating Manual, 4th Ed., 1978. (v6)' R. D. Swisher, Surfactant Biodegradation, pages 16-17 and 147, Marcel Dekker, Inc., 1970. (7) D. Li.u, Study on Biodegradati.on of Ani.line and Marlon A, Biodeterio^r'Iamtion 5, Edited by T. A.` Oxley and S. Barrrv, 1983. 000492 Form 1062-8-A-PWO Sample Description f Ax Environmental Lab -- Work Sheet YluJKu^J' .3LLab Request No Date , 7 A / f r 3 Analyst:. U M . F i l l Caas-It, QW -V O L- coi'Hv D( R^O I^ w t __ M j S O y 1^ >w( pit C-li ^cr^iJ^tr^ i0) jy\) S/ux&g-*v 0\ (U^Cit-- *ia> 1^? 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