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BIODEGRADATION (BOD/COD) TEST SUBSTANCE Identity:A mixturecontainingperfluorooctanesulfonatweh,ich may alsobe referredtoas PFOS, FC-95 or as a component of FC-201 AF. (1Octanesulfonicacid)(CAS # 2795-39-3). Remarks: The 3M productionlotnumber was not noted. The testsample isFC-201AF (L-13652). Currentinformationindicatesitisa mixtureof3% PFOS, 18.59% diethyleneglycolbutylether,37.81% water,14% ethylene glycol,8.25% Acrylicfoamer,9% sodium octylsulfate0,.3% sodium lauryl sulfate3,% tdethanolamine,6% sulfbnatedalkylethersalts,and 0.05% tolyltriazole. The followingsummary applies to a mixture with incompletely characterized concentrations of impurities.Data may not accurately reflectthe biodegradabilityof the tluorochemical component of the test sample. METHOD: Method: Not given Type: Aerobic GLP: No Year completed: 1996 Contacttime: 28 days lnoculum: Not given. RESULTS Chemical Oxygen Demand (COD): 1,710,000mg/kg BiochemicalOxygen Demand (BOD): 5-Day: 10-Day: 20-Day: 28-Day: 265,000 mglkg 288,000 mg/kg (replicate) 385,000 ffig/kg 382,000 mg/kg (replicate) 494,000 mg/kg 501,000 rngtkg (replicate) 508,000 rrQ/kg 504,000 mg/kg (replicate) CONCLUSIONS No conclusionsgiven. Submifter: 3M Company, EnvironmentalLaboratory,P.O. Box 33331, St. Paul,Minnesota,55133 DATA QUALITY Reliability:Klimischranking3. Study lacksdescriptionand recordsofthe method followed.The inoculumwas not properlycharacterized.Sample puritywas notpropedy characterizedand the study lacksanalytical confirmationofthe amount offluorochemicalproportioninthe solution. REFERENCES This studywas conducted by Pace AnalyticaSlervicesofGolden Valley,MN atthe requestofthe 3M Company, Lab Request number N3747, 1995. OTHER Lastchanged: 6/26/00 06/25/2000 ENVIRONMENTAL LABORATORY ARCHIVED FINAL REPORT LAB REQUEST NO. N3747 REQTJESTOR NAME: SBS/Shari Loushin DEPARTMENT: 3058 PRO,JECT NO: BILTWENVIR DATE RECEIVED: 11/30/1995 DESC: FC-201AF Light Water BOD (L-13652) CONTRACT LAB(S): PACE EXP COMP DATE: 01/04/1996 DATE COMPLETED: 02/06/1996 PROJECT LEAD: TL HATFIELD PHONE NO: 651-778-7863 3M FAX NO: 651-778-6176 Aquatic Tox testing results: See LR N3281 for algae, and N2964 for fish, daphnia, microtox and sludge respiration inhibition. sab 11/30/95 Sample dilutions depleted after 10 days for bod. Sample will be re-set at lower concentrations 1/5/95. mjc pace 1/2/95 -------------------------------------------------------------------------------- SAMPLE DATE CODE DESCRIPTION RESULT MDL or (95% C.I.) -------------------------------------------------------------------------------- 1 09/04/95 FC-201AF Dark Liquid PACE COD PACE P-CBOD-05 PACE P-CBOD-10 PACE P-CBOD-20 PACE P-CBOD-28 2 *COD *BOD-05 *BOD-10 *BOD-20 *BOD-28 (CARBONACEOUS) (CARBONACEOUS) (CARBONACEOUS) (CARBONACEOUS) 1710000 MG/kg 265000 mg/kg 385000 mg/kg 494000 mg/kg 508000 mglkg DUP #1 ------------ PACE P-CBOD-05 PACE P-CBOD-10 PACE P-CSOD-20 PACE P-CBOD-28 *BOD-05 *BOD-10 *BOD-20 *BOD-28 (CARBONACEOUS) (CARBONACEOUS) (CARBONACEOUS) (CARBONACEOUS) 288000 382000 501000 504000 mg/kg mg/kg mg/kg mg/kg * = CONTRACT LAB DATA 1000 14000 14000 14000 14000 14000 14000 14000 14000 Product Testing Modifled CBOD Test 5, 10 ,2C & 28 Day Analyses PACE Sample No. ProductID C) /C) PreparatioonfStockSolutionofProduct (NominalConcentmbon 1500 nVL) Sample 1 Weight ofProduct 5co7 grams Diluteto1 L. ConcentratioofnStockSoluton 1500.')mg/L Make a 1:10 dilution. ooo mLs dilutetdo Qoo O-mLs 10 0 o -R- FinalWorking Solu@onConcentration 15c). M91L PACE Sample No. ProductID p 10/1- PreparatioonfStockSolutionofProduct (NominalConcentratio1n500 mg/L) Sample 2 Weight ofProduct 1, 500-7 grams Diluteto1 L. Concentra@onofStockSolubon 1-500.-7 mg/L Make a 1:10 dilution. .200 mLs dilutedto OOOC) mLs /are /0-0 --Q FinalWorking SolutionConcentration 5(> o? mgfl PACE Sample No. 3 ProductID -7. PreparationofStock Soluton ofProduct Sample 3 WeightofProduct 0. -7 y @ Fgrams DilutteoI L - Concentrafloonf StockSolution Make a 1:10 dilubon. Q c>o mLs dilutedto @i Q 0-ru@ Final Working Solution Concentrabcn- (NominalConcentration1500 mg/L) mg/L mLs 166 -7q.99 m[L Produc-tTesting 14odiFiedCBOD Test 5,10, 20 & 28 Day Analyses QC Data Sample Product CBOD Day Dii No. ID Results No (mgtl) seed Vol (mL) Inhib. Samp YIN Vol ? (mL) 00 Drop ir,.t,al Final DO Drop irit,-al arnp Dissolv Dissolv, Initi-al Final- Dilul!on Conc. Oxygen Oxygen Final Seed Cor Results (mg/L) (mg[L)i(mg[L) (mg[L)l(mg/L)I(mg/L) 5 Day Blank<= 0.5mg[L 5 Blank <= 0.5 mg/L 0.13 5 Seed lnh. 0.714 5 Seed Inh- 0.608 0.661 5 Seed 0.582 5 Seed O@604 0.593 5 LCS inhib 166.95 5 LCS inhib 143.95 155 LCS 171.85 5 LCS 222.85 197 5 Toxic@y Blank 389.7 5 ToxicityBlank ToxicityBlank 529.7 5 1 748.7 5 'whereSeed Volisthe5 mLs ofseed inear-hlestflask N 9.01 8.86 N 8.97 8.86 25 y 8@97 5.40 25 y 8.97 5@93 25 8.99 6.08 25 N 8.97 5.95 5 N 8.97 4.97 5 N 8,97 5,43 5 y 8@98 4,95 5 y 3 8-'j7 392 5 y 100 8.08 3.59 5 y 100 8.31 2.42 5 y 100 8.29 0.21 0.15 0.11_ 3.57 3.04 2@91 3-02 4.00 3.54 4.03 505 4.49 5.89 8.08 3@57 304 2-91 4284 3548 3492 3.02 36@24 3.34 13339 0 2.88 28790 344 3-'370 4.46 44570 390 389,70 5@30 7.49 52970 74870 10 Day QC Blank Blank Seedlnh. Seedlnh. 10 0.54 10 1.15 10 0.88 1.02 1 20 Day QC Blank Blank 20 0.31 20 Seedinh. Seed lnh. 1.37 1.01 20 1.19 20 28 Day OC N N y y Y 25 Y 25 8.44 8.46 3.20 ArM 8.67 8.69 2.13 3.92 0.57 0.51 5.77 AAJ 0.34 0.28 6.84 5.05 5.77 69.2244 92 =7 4.41 5522.92 6.84 8208 5.05 6060 i[-- Blank<= 1-5 mgfl 28 N Blank 0.47 28 N Seedinh.* 1.50 28 y Seedlnh. 1.13 3 2 2 *8 y 8.5 0.51 8.54 0.43 1.47 7.50 7 50 90.00 565 6780 The ToxicityBlank contains sample at th6 highestconcentrationused fordilutions1,0 mg/L and i6r'eemLs of.Hach ILCS sti@6ard-,.'@@'H.a!cThhe standard is twiceas .oncentratedas the method Hach standard is twiceas concentrated as the method GGA standard ancfther@forethe fi@n.1rem6ssutlbte dividedby 2,in-orderto evaluateagainstthe 198 +f-31 criteria @M Sio Date: IroductTesting Time: -lodifleCdBOD Test Analyst. 10, 20 & 28 r-)aAynalyses Reviewe &- DO Drop ample 3 ample No. and IroductID CBOD Day Results -(mgfkg) 0 Oil Seed lnhibSamp Samp Seed No. Vol YN Vol Conc. Corr. (mL) 7 (mL) (mg/L) 1 5 Y 100 25 Initial Dissolved Oxygen (mg[L) 8.14 Final Dissolved Oxygen (mq/U DO Drop Initiamlinus Final (mg/L) initiamlinus Finalminus Seed Corr (mg[L) Dilution Result (mg/L) -c6077.0 0 2 5 Y 50 12.5 8.62 N3747-1 0 1 3 1 5 Y 35 8.75 8.80 Repeat 0 1 4 5 Y 20 5 5 1 5 Y 1()0 25 0.661 '6489638 178276.8 5 2 5 Y 50 12.5 0.661 290664.4 5 3 5 y 35 8.75 0.661 8.84 0.22 3.50 3.05 7.92 5.12 5.75 7.26 4.46 5.09 26.75 43-62 26,rCOO )32574-8.0 5 4 5 Y 20 5 0.661 4.92 3.92 3.26, 48.89 10 1 5 Y 100 25 1.02 0.12 8.02 --7.00 385320.18 10 2 5 Y 50 12.5 1.02 383820.9 10 3 5 y 35 8@75 1.0129 385000@_.S86819.51 10 4 5 Y 20 5 1.029 0.12 1.06, 3.95 8.50 7.74 4.89 7.48 6.72 3.87 57.60 58.05 20 1 5 y 100 25. 1.19 0.08 8.06 20 2 5 Y 50 12.5 -1.19 0.11 8.51 49ACOO 493769.6 5 Y 35 8.75 1.19 5 Y 20 5 1.19 0.11 2.71 8.69 6.13 4.94 74.10 28 1 5 Y 100 25 1.322 0.09 8.05 28 2 5 Y 50 12.5 3111*-.'2001:3@392 28 3 5 Y 35 8.75 i'13.232 5080001 507763.0 28 4 5 Y 20 .5, 1.3322 0.11 0 .12 2.44 8.51 P-68 6.,--5.081 7=6. 20 -S SC)D (mg/L) {(LCS DO Drop - Seed CorrFactor) X 300 mL ILCS Vol (mL)j 12 eed CorrectionFactor(mgfl) Seed ControlDO Drop X 1(3001 Seed OilVol (mL)) X (SmL*'/3DO mL) where 5 mL isthevolume of seed used inthe testflask I I @-@00(mgag) Samp DO Drop -S eed Corr Fa cior) X (30 r;L I-S,a,mpl ternativetlhyeCBOD (mglkg)may be calculateads felOlws: Vol (mL)'X (10 0 ' io, .. . mL I Sar r.p VA. (g))X (gXL/kgXmL) BOD.(mg,lkg) Samp 00 -Drop (mg/L)@ Samp C.one (mg/'Li );@-i".660',6(g)',O"M' 3m Bio Date: C) Product Testing Time: Modified CBOD Test Analyst: ,@fc- 5, 10, 20 & 28 Day Analyses Reviewed: DO Drop Sample3 OUP Sample No. CBOD Day and Results ProductID (mgtkg) Dil Seed InhibSarnp S-P Seed No. Vol YIN Vol Conc Corr. (mL) ? (-L)(mg)L)Factor Initial Dissolved Oxygen frng/L) Final Dissolved Oxygen fmg/L) @10 Drop Initiamlinus Final (mg/U Initiamlinus Finalminus Seed Corr (mgfl) 01 5 Y 100 25 8.19 356077.0 0 2 5 Y 50 12.5 8.70 N3747-1 0 3 5 Y 35 8.75 8.74 Repeat 0 4 5 Y 20 5 5 1 5 y 100 25 0.661 288045.58 281428.67 5 2 5 Y 50 12.5 0.661 29466',1.49 5 3 5 Y 35 8.75 0.661 U.15 1.00 2.92 8.04 7.70 5.82 7.3 7.04 5.16 ("288000 Icz-@ 54 10 1 5 Y 20 5 y 100 5,0.661 251 1.02 6.74 0.12 2.07 8.07 1.41 7.05 382036 10 2 3712!-)53 10 3 3928167 10 4 5 Y 50 12-5 1.02 5 Y 35 8.75 1.02 5 Y 20 5 1.02 0.12 1.22 3.86 3.58 7.52 4.95 7.56 6.50 3.93 20 1 5 Y 100 25, 1.19 0.09 8.10 20 2 5 Y 50 12.5 @1.19 0.09 8.61 20 3 501000 500766.3 20 4 5 Y 35 8.75 1.19 5 Y 20 5 1.19 0.10 2.61 8.64 6.20 5.01 28 1 5 Y 100 25, @1.32 0.11 8.08 28 2 5 50 12.5 1.32 0.11 8.59 28 3 5 Y 35 8.75 1.32 I 504CO01 5037(>4.9 28 4 5 Y 20 5 1.32 0.11 2.45 863 -6.36 5.04 Dilution Result (Mgfu 42.23 44.22 55.71 58.9 5 75.15 LCS BOD (mgll) ((LCS DO Drop -Seed CorrFactor) X 1300 mL ILCS Vcl (mL)l )12 Seed CorrectioFnactor(mgll) Seed ControlDO Drop X (300 1Seed DilVol (mL)) X.(5mL**1300 mL) where 5 mL isthe volume of seed used inthe testflask CBOD (mgag) Samp DO Drop - Seed Corr Factor)X (300 mL 1,SampiVol (@nL,)X)(1000 mL I Samp VA. (g))X (gXLfkgXmL) Alternativ3ltyhe CBOD (mg,lkglma@ be calculatedas folows,,,, CBOD (mglkg) ISamp 00 Drop (mg/L) /,SampConc img/L) X 1,000,000 mg,'kg