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BIODEGRADATION (OECD 301 E) TEST SUBSTANCE Identity:A mixturecontainingperfluorooctanesulfonatweh,ich may alsobe referredto as PFOS, FC-95, or as a component of FC-203. (1Octanesulfonicacid)(CAS # 2795-39-3). Remarks: The 3M productionlotnumbers were Antwerp,Belgium 9/82 and US 3072. The testsample isFC-203 produced inAntwerp, Belgium. CurrentinformationindicatesFC-203 isa mixtureof 1.34% PFOS, 35% diethyleneglycolbutylether,37.85% water,20% ethyleneglycol,2.66 % Sultonefoamer, 3% sodium octylsulfate0,.1% sodium laurylsulfatea,nd 0.05% tolyltriazole. The followingsummary applies to a mixture with incompletely charactedzed concentrations of impurities.Data may not accurately reftct degradation potentialof the fluorochemical component of the testsample. METHOD Method: ModifiedOECD Screening Test,OECD 301 E,with DOC Analysis Test type: Ready Biodegradability GLP: No Year Completed: 1983 Analyticalmonitoring: Dissolvedorganiccarbon (DOC) Statisticamlethods: Resultswere determinedby calculatioonfthe % DOC removal and graphicinterpretation. Test organism source: A 50:50 mix ofsoilextractand secondary effluent. Fresh sandy loam agriculturasloilsfrom Ramsey and Washington Counties, MN. Secondary effluents,upernatantofactivatedsludge mixed liquor aerationbasin,obtainedfrom Metrow Wastewater Treatment Plant,St.Paul, MN. Test condition: Dilutionwater: Deionized water Miner-alNutrient Medium: OECD medium using yeast extract,OECD medium using syntheticvitaminsolutionand OECD medium with reduced nitrogencontentbut usingyeast extract. Reference and testsolution preparation: Test and reference solutionswere preparedforeach ofthe threemineralnutrient mediums, except US 3072 onlyinOECD withyeast extract.Solutions were splitintoaliquotsand put intoEdenmeyer flasks.Test materials preparedto givefinaltestconcentrationof40 mg DOC/L, reference standardsat20 mg DOC/L and 15 mg DOC/L forsodium benzoate and LAS respectively. Test vessels: One L Edenrneyer flaskscontaining500 mL test solutionand capped withfoam plugs. I Incubation conditions; Continuous dark conditions Temperature: 23.5 - 24*C Agitation: Continuous Number of concentrations: One plus references and blank, al in duplicateforeach nutrientniedium type. lnoculum condition on testinitiationN:ot taken. Element Basis: Decrease indissolvedorganiccarbon compared to blanks. Test substance flasks conditions: Not recorded. RESULTS Nominal concentrations: Test materialsat-40 rng DOC/L, sodium benzoate at-20 mg DOC/L, LAS at-15 mg DOC/L and Blank controls. Element 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) Remarks: Testingwas conducted on the mixtureas describedintheTest Substance Remarks field.The values reportedapplyto thatmixtureand not the fluorochemicalproportionalone. CONCLUSIONS FC-203 Antwerp 9/82,mean degradationbased on DOC removal ranged from 35% forthe low nitrogenseriesto 94% forthe yeast series,with89% mean DOC removal forthe vitaminseriesafter28 days. FC-203 US 3072, degradationbased on DOC removalwas 97% after28 days. Submitter: 3M Company, Environmental Laboratory,P.O. Box 33331, St. Paul,Minnesota,55133 DATA QUALITY Reliability:Klimischranking= 2. This study meets the criterifaorquality testing.However, the sample puritiewsere not properlycharacterizedand the study lacksanalyticaclonfirmationofthe amount offluorochemical proportioninthe solution. REFERENCES The studieswere conducted by the 3M Company, EnvironmentalLaboratory, 3M Lab Request number 9611, 1983. OTHER Last changed: 6/28/00 F ofm 6747-11-D TECHNICAL REPORT SUMMARY TO: TECHNICAL COMMUNICATIONS CENTER - 201-2C-12 (Importan-t Ifreporitsprinteodn bothsideosfpaper,sendtwo copiesto TCC) Guidelineosn reversseide. Division Fnuirnnmpnt-al Project T.ahnrat-nry (PP. & Pr) qt- Paul, Minnesota Dept Number 053.-5 r a t, onal- Flogpig 't@,m@rn MndifiAd To aRrT) gnrppning Tpgt nn Fr-201, Fr-201A, and vr-f;()() ItOO3 Period Covered or Date 'AM rpr-man3Z 'O'it-olnq3Z' 7 _/ F-mployeal4@Nu@tr(.) N @i.-bo oA ,.nc;pe ,,,ironmpnt-ai T-ahnralrnrU - 7l-2W-tlg; 47816 No. of Pages Including Covershost NnnP- - qpp Fnvirnnmpnt--;%l T.ah Reauest :19 11 1 1 z-- SECURITYIO-Q OpenReportS&ummary[ICloseRdeport-OpeSnummary 3M CHEMICAL b,,[ICheckboxifnowchemicaalrsereportUesde.ChemiREGISTRY P' calRegistFroyrm6092torepoarltnlewsubstances. KEYWORDS: LabCode CURRENT OBJECTIVE: To test the repeatability of the modified OECD Screening Test in measuring the biodegradability of Light Water OtheKreywords products. REPORTABSTRACT:ThisabstraicntformatiisdoinstribubtyetdheTechnicCaolmmunicatiCoennstetroaler3tM'ertso CompanyR&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)'@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 prdducts are readily biodegradable. cc: R.L.Bohon-21-2W-05 D.R.Ricker-235-lB-10 D.W.Kent-236-2A-04 lnformatioi,spoynl. Initials: 3M CONFIDENTIAL 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? 1 Laboratory showed that three L/W products were highly biodegradable 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 1 Results of 1980 Testing on Light Water Products Product 7 1 FC-203 NFP 13 FC-206 23 FC-3.017 2 37 Hydroquinone 3 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 FC-3017 is freeze protected FC-206. 3 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 for FC-206 in the 21-day long TOC Degradation Test contradict his own BOD /COD data. His 5-day biochemical oxygen demand 5 (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 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 30 C-BOD 20 Lab (mg/ia) (mg/k (mg/kg) co COD 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. 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 0.78 .92 Average S. D. 325,000 338,000 396,000 .81 .83 73,000 57,000 33,000 .16 .11 FC-780B Lot 501 3M Pace Serco Capsule 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 S. D. 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@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 lolution 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 boc 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 extra,ct 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. Th-e 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(gyescribed by the manufacturer of the organic carbon analzyer. 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 screening Page 5 July 9, 1984 Biodegradation Table 3 of LIGHT WATER Products and Refernce Materials Product/Vitamin Source Sodium Sodium Sodium Sodium Mean Benzoate/Yeast-1(1) Benzoate/Yeast-?,, Benzoate/Vit.-l'*@' Benzoate/Vit.-2 (3) FC-203 /Yeast-1 FC-203/Yeast-2 FC-203/Vit.-l FC-203/Vit.-2 Mean U.S. FC-203/Yeast-1 U.S. FC-203/Yeast-2 Mean FC-203A (5) /Yeast-1 FC-203A/Yeast-2 Mean FC-600 3 /Yeast-1 FC-600/Yeast-2 Mean LAS/Yeast-1 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 95.3 92.1 83.6 95.2 92 79.2 90.7 95.5 96.0 96.5 97.5 97 11.0 85.1 86.4 92.5 87.2 96.0 92 76.3 89.3 87.0 94.2 88.8 91 25.1 20.4 30 --to) 49.:r-' 29.7 52.1 33.4 43 Footnote S. (1) Used yeast extract as vitamin source. (2) Used OECD synthetic vitamin solution as (3) )From Antwerp 1982. (4 17-day samples were only taken for LAS. (5) From Antwerp 1980. originally labelled (6 Sample contaminated, not used. vitamin source. FC-203 NFP. ki-yuj-u 1. READY BIODEGRADABILITY:ModLfLed S'CreenLngTe OECD 301E -- Ado ted 12 Ma@ 81 EnvLronmentaL Lab Request No. 9611 100 THIS SERIES WHS RUN USING 90 'STHNDHRD, NUTRIENT SOLUTION 000 CONTAINING YEAST EXTRHCT. m . ................................................................................................... 70 .........................................................................................*.................. cr_ CC3 40 ...... C9 ELI C03 30 m %oooolooo 20 ..../................. 10 7 ......................../......................... Legend ..........................................x...... 0 ro--m, E3 M 2"0, rc-ow, 14 21 28 MYS Figure 2 RE ADY BIODEGRADABILITY: ModLfLed ScreenLng T OECD 301E -- Ado ted 12 Ma@ 81 EnvLronmenta@ Lob @equest No. 9611 100 THIS SERIES WAS RUN USING 90 STANDARD NUTRIENT SOLUTION WITH VITRMIN SOLUTION. 00 ............................................................................................................................... c:) n C:) ...................................................................................... C3 50 a: C3 40 .................................................................................................................... cr_ w C-9 w C3 3o 0 m 20 ................... ................................................................................................ Lege 10 A sooiu X FL%--20 0 ...... 0 7 14 21 @DRYS Figu re 3 READY BIODEGRADABILITY: ModLfLed ScreenLng T OECD 301E -- Ado ted 12 MaS 81 EnvLronmentaL Lob Nequest No. 9611 100 90 80 cr_ c:) THIS SERIES WAS RUN USING 'STHNOARD' NUTRIENT SOLUTION CONTAINING YEAST EXTRACT. ............................................................................................................. 0 ....................................................00.......................................... Z 50 cr_ C3 40 ...........................@...o............I..................9......................0..........0......................................... cr_ C9 LL3 C3 C) m 20 ........oo.................o...:./..........o...o............o....o....................... Legend 10 FO@-2M, FC-203 7 14 21 J)HYS l@'jy.u i-u 4 READY BIODEGRADABILITY: ModLfLed Screen'ung I OECD 301E -- Ado ted 12 Ma@ 81 EnvLronmentaL Lab equest No. 9611 ioa THIS SERIES WAS RUN USING 'STHNORRO*-NUTRIENT SOLUTION CONTAINING YEAST EXTRHCT. so THE LAS REFERENCE WAS DILUTED WITH FRESH NUTRIENT SOLUTION 00 ON TEST DAY 29 AND RE-INOCULATED. cr_ Ca 70 C.3 - ------- C3 cr. Ccr3_ 40 ................ C!D C3 30 m 20 ....... 0 ...... 7 ---------- 14 21 SORYS ....... -- ------- ------- -------- Legend I& us lumem co DIU)= L9s mr 20 35 42 OE CD Screening Page 9 July 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 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/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',',,, concentration @6 . 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 larlon A (dodecylbenzene t7 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. OECD screening Page 10 July 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 carF'lw-ed-outby 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 (Der TOC Abbautest - ein Verfahren zur Prufung von organbisch7en Substa'nzen auf Vollstandigen 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. Form 1062"-A-PWO Sample Description At t EnvironmentaLlab - Work Sheet Lab Request No. Itto Date: -7 Analyst. ",OLV6 I Cl t) 7- Ff-U qL C.,,+4, ..................... v.J 411,ts Zx A-,(ct q, 0 L Forrn'lOi2O.8.A-PWO Sampi a Description u- P/ti, 10 0. EnvironmentalLab - Work Sheet Lab Request No.. Date: Analyst:_iu a FC- -L L4+ 30 FC-- 2.03 (0@wiweiar -4/fzl) (AA-r(Jir-_Rlfito Mf P) u ("Twelee!2Ll%,r2 V OF IA Form ICr220-8-A-PWO SampleDescription Lab RequestNo. Environmental Lab - Work Sheet Date: &--2- Analyst:&), I 44::ax v C;/ i@T Ae - 0( 17 I, L7 '.germ10320- EE & pC DedicatedTo Quality EnvironmentalService Sample Des Form 24698-PWO IV lset Lab Request No. Date: Analyst: C;/ 0/t@e D 5 I-As - I 7Z/L@o@ Fo.rn 10620.8-A-PWO Sample Description EnViro!M v Work Shoot Lab RequestNo. 49(o Date: e?-2- Analvst: e!;-, C;/ YAP 577,1@,uOjteD" e4,LR&, N7- &f -4-f@ Lr 12 S-,31<- ;L I S- -.45 i@ Lo. I ph t bm t SO e ds VP,422 AL.-I, dzm" dew a cl, -Form 105204-A-PWO Sample Description D, r EnvironnwntalLab - Work Sheet Lab RequestNo. Date: Analyst:ZA e@; C/ A-e- 57@'Iou0/te D 2od@@ .4A J-dz4w Aa 44=44 A::3@C- 4 col C/ da 61 iEAVr 4,0 Form 10620-8-A-PWO Semple Description A 6 @i@z -1@ EnvironmentalLab - Work Sheet Lab Request No. Date: Analyst: 0 I 30/F-/ 17z@ f (e4-i 11; Y21-x@ 40-4t&4-@v 7A /V-44ail 44 7 Forr@ IM2 0-8-A-PWO Samp'le Description EnvironmentalLab - Work Sheet Lab RequestNo.-2@Z/- Date: Analyst: -7 u (,4 AOa-c-CUcv,e- 7o @/Xk lei, 17 L BIODEGRADATION (BOD/COD) TEST SUBSTANCE Identity:A mixturecontainingperfluorooctanesulfonatweh,ich may also be referredtoas PFOS, FC-95, or as a component of FC-203. (1Octanesulfoniaccid)(CAS # 2795-39-3). Remarks: The 3M productionlotnumber was notnoted. The testsample isFC-203. Currentinformatioinndicatesitisa mixtureof 1.34% PFOS, 35% diethyleneglycolbutylether,37.85% water,20% ethyleneglycol,2.66 % Sultonefoamer, 3% sodium octylsulfate0,.1% sodium laurylsulfatea,nd 0.05% tolyltriazole. The followingsummary applies to a mixture with incompletely characterized concentrations of impurities.Data does not accurately reflectthe degradation potentialof the fluorochemical component of the testsample. METHOD: Method: COD by EPA 410.1 and CBOD by EPA Type: Aerobic BOD and Dichromate RefluxCOD GLP: No Year completed: 1991 Contact time: 20 days lnnoculum: Source notgiven 405.1 RESULTS Chemical Oxygen Demand (COD): Carbonaceous BiochemicalOxygen 5-Day: 1O-Day: 20-Day: Demand 1,100,000 mg/kg (CBOD): 630,000 mg/kg 880,000 mg/kg 1,100,000 mg/L Remarks: Testingwas conducted on the mixtureas described inthe Test Substance Remarks field.The values reportedapplyto thatmixtureand not the fiuorochemicalproportionalone. CONCLUSIONS No reliablceonclusionscan be derivedfrom these studies.The indicatioins thatthe majorityofthe productcomponents are readilybiodegradable. Submifter: 3M Company, EnvironmentalLaboratory,P.O. Box 33331, St. Paul,Minnesota,55133 DATA QUALITY Reliability:Klimischranking= 3. The inoculum isnot propedy characterized.The testingwas conducted on a mixturewithchemicals having varyingdegrees ofbiodegradabilitlye,adingto potential misinterpretatiofnthe results.The sample puritywas not properly characterizedand the studylacksanalyticaclonfirmationofthe amount of fluorochemicalproportioninthe solution. REFERENCES The studieswere conducted by Pace IncorporatedM,inneapolis,MN atthe requestofthe 3M Company, 3M Lab Request number J2176, 199 1. OTHER Last changed: 6127/00 ace. ....%.it.0'QUA'"' REPORT OF LABORATORY ANALYSIS August 13, 1991 Mr. Wade Schoil 3M Environmental Laboratory 935 Bush Avenue Bldg. 2-3E St. Paul. MN 55133 RE: PACE Project [4o. 910711.501 J2176 -74f 4At/'90 "*44 Dear Mr. Scheil: EnclosedIs the report of laboratoryanalysesfor samples received July 10, 1991. If you have any questionsconcerningthis report,pleasefeel free to contactus. Sincerely, iisa A. Arndt Project Manager Enclosures 1710 Da*s D*os WO wav@Pft m $6422 TIL,9124W46U3 FAL-612-US-nl? nil sw** mmompsk vim" 1To*%am* IN" cityb.wo So Ftw4ismC,dlo* K@ C".1- In&IpbsC,alhr* owbm mw* Cwdm A*mftN" Cw*a NowVailN.ew Ywh Rttobwsfktmplva* 0~, Cdwaft AnEOW OffwWft plo ace. I"IA%SU4 A%Ci 0- QVA I. Mr. Made Scheil Page 5 J2176 PACE Sample Number: Date Collected: Date Received: Parameter INORGANIC ANALYSI INDIVIDTJAL PARAMETERS Biochemical Oxygen Demand, Carb 05 Day Biochemical Oxygen,Demand. Carb 10 Day Biochemical Oxygen Demand, Carb 20 Day Chemical Oxygen Demand REPORT OF LABORATORY ANALYSIS August 13, 1991 PACE Project Number: 910711501 Units 10 0245070 07/09191 07/10/91 MDL J2176-5 DATE ANALYZED & MET mg/kg mg/kg mg/kg mg/kg 6000 6000 6000 50000 630000 880000 1100000 1100000 07/19/91 07/19/91 07/19/91 07/25/91 EPA 405.1 EPA 405.1 EPA 405.1 EPA 410.1 MDL Method Detection Limit 1710Ono" 064 W* MNWPds. N 55422 TIL.slz44"543 FAL-812-525-"77 onim swft mwwwk Mmmsm q-.,ToRm FW* r.-@47@ so fram*mCdfwWo Km Cky,NUIA Cbwbft M" Car" AAVft ft* Carob@ NowYak Now Ywk Fktibm P@lip" Dmw. Cdwsb EOW oppwuwayEw#bw we ac Mr. Wade Schell Page 6 J2176 PACE Sample Number: Date Collected: Date Received: Paramet r INORGANIC NALYSIS INDIVIDIJAL PARAMETERS Biochemical Oxygen Demand, Carb 05 Day Biochemical Oxygen Demand. Carb 10 Day Biochemical Oxygen Demand. Carb 20 Day Chemical Oxygen Demand REPORT OF LABORATORY ANALYSIS August 13, 1991 PACE Project Number: 910711501 10 0245089 07/09/91 07/10/91 unw _MQL JILUL--k- DATE ANALYZED & METH mg/kg ig/kg Mmg/kg mg/kg 6000 6000 6000 50000 390000 830000 890000 1000000 07/19/91 07/19/91 07/19/91 07/25191 EPA 405.1 EPA 405.1 EPA 405.1 EPA 410.1 MDL Method Detection Limit These data have been reviewed and are approved for release. )tL Starla Enger Inorganic Chemistry Manager II10DevoDnrifMt" mmampok m SS422 TFL'61244"U3 FAL'812-525-3377 offew sem* mwmsspok mwmwu Tav^ FbrWo bm Ckl.bwo Chobta,N" Co" Alhwft N" Coda NM TWLUM Vwk So Ffwzim,CdkffAt Kmm CkyW,mowl Pktskv* Pwm*mb Dww.Cdweb taAMPIMCAOWS'.-! Aatpd Dpwuw* Emolo