Document Qkr28b8zYYJow4v4XL3xZmNbo

/ ft m -o M 0 5 BIODEGRADATION TEST SUBSTANCE Identity: Perfluorooctanesulfonylamido(ethyl)acetate; may also be referred to as PFOSAA, FC-128 or as the major component of FC-127, FC-129, FC-109, FC-109-X or R1904. (Glycine, Nethyl-N-[(heptadecafluorooctyl)sulfonyl]-, potassium salt, CAS # 2991-51-7) Remarks: The test sample is FC-129. The study-defined composition is 50% Potassium fluoro alkyl carboxylate, 18% butyl carbitol, 28% water, and 4% ethanol. This is a minor contradiction to the formulation available from proprietary 3M databases indicating it is a mixture of 42% test substance, 32% water, 14% 2-butoxyethanol, 4% ethanol, and 8% C4-C7 fluoroalkyl carboxylate compounds. Test material was from 3M Deutschland production batch 2304. The following summary is abbreviated because the test sample is a mixture of the test substance in a water/organic solvent solution. Data does not accurately relate biodegradation of the test sample with that of the test substance. METHOD: Method: OECD 301E Type: Aerobic GLP: No Year completed: 1984 Contact time: 28 days Inoculum: Secondary Effluent of a domestic sewage plant RESULTS Mean DOC removal after 28 days: 90% Remarks: Organic carbon content of the test material was determined to be 13.5 mg/100 mg sample by a carbon analyzer. CONCLUSIONS No reliable conclusions can be derived from this study. Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 000367 DATA QUALITY Reliability: Klimisch ranking 3. The digestive procedure of the instrument used in this study to determine TOC is not aggressive enough to break the carbon-fluorine bonds. The TOC is therefore inaccurate. The calculated TOC is 22% compared to the 13.5% obtained by analysis. These results are expected to be representative of the organic solvents present and not of the Perfluorooctanesulfonylamido(ethyl)acetate. Lack characterization of test substance and confirmation of test concentrations. REFERENCES This study was conducted at Research and Consulting Company AG, Ch4452 Itingen / Switzerland at the request of the 3M Company. OTHER Last changed: 5/17/00 000368 Internal Correspondence ce: R. L. Bohon - 2 1 - 2 W - 0 5 To: From: Subject: Date: D. R. R I C K E R - C O M M E R C I A L C H E M I C A L S DIV. - 2 3 6 - 1 B - 1 0 E. A. R E I N E R - E N V I R O N M E N T A L L A B O R A T O R Y / E E & PC - 2 1 - 2 W - 5 OECD BIODEGRADATION TESTS ON AND FC-170C O C TO BE R 24, 1984 We have received copies of the OECD Screening Tests on FC-129 a n d F C - 1 7 0 C f r o m D. R e e s e of 3M G e r m a n y . The results o the FC-129 study incorrectly indicate that this product is readily degradable. This result does not accurately represent the actual susceptibility of this product to b i o d eg ra da ti on 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 inst ru me nt used in this study is not strong e n o u g h to brea k fluorine-carbon bonds. Therefore, these results, really only show that the butyl Ca rb it ol and ethanol in this pr od uc t are biodegradable. The results of the FC-170C study are more useful but still * inaccurate. These results confirm our previous BOD 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 mo le cu le is al m o s t c e rt ai nl y not biodegraded. The data in these reports confirm the inability of the UVpersulfate digestion method used to degrade the perfluorocarbon portion of these products. The measured TOC for FC-170C was 24 mg C per 100 mg product while the calculated TOC based on formulation information is 38 mg C per 100 mg product. The measured TOC for FC-129 was 1 3 . 5 % ; its calculated TOC is abou t 2 2 % . Because of the weak and inappropriate TOC method used, we are not going to add these results to our Product Envi ro nm en ta l Data Sheets. Customers and regulatory agencies would likely misinterpret these results and think that these products are more biodegradable than they actually are. EAR/mb Attachment: OECD Screening Tests on FC-170C and FC-129 000369  f - {.7 f u r ~ R E S EJk R C H RCC ft C O N S U L T I N G 1 (4 ** COMPANY AG s\ . r - ^ M 1-" PROJECT 034244 READY BIODEGRADABILITY: MODIFIED OECD SCREENING TEST FOR FLUORAD /FC-129 3V REPORT P.O. Box CH-4452 Itingen Switzerland Phone 061 / 98 52 52 Telex 966 136 RCC CH 00037Q __ RCC PROJECT 034244 FLUORAD FC-129 CONTENTS PREFACE 1 INTRODUCTION 2 MATERIALS AND METHODS 2.1 Chemicals 2.2 Experimental design 1 3 RESULTS 3.1 Degradation of testcompound 3.2 Degradation of standard compound (aniline) 4 CONCLUSION 5 REFERENCE 6 TABLES AND FIGURES rA>. Page 3 '4 4 4 4 5 5 5 5 5 6-11 v* f 000371 RCC PROJECT 034244 FLUORAD F-129 PREFACE Project Sponsor Study monitor 034244 3M Deutschland GmbH Postfach 643 D 4040 Neuss 1 D. R e e s e 3 Testing facility Study director RCC Research and Consulting Company AG CH-4452 Itingen/Smitzerland Dr. H. Ellgehausen' Date-. S e p t e m b e r i9, 1984 / hoh T e c h n i c a l a s s i s t a n c e ^ - 0. U u e t h r ich Start of experiments A u g u s t 17, 1984 Date of completion r i' S e p t e m b e r 14, 1984 Archiving Raui data, p r o t o c o l , report, d u p l i c a t e of report-. RCC Research and Consulting Company AG CH-4452 Itingen/Suiitzerland 000372 RCC PROJECT 034244 FLUORAD FC-129 4 X INTRODUCTION The objectives of the present test mere to fallow the b i o d e g r a d a b i l i t y of F L U O R A D F C - 1 2 9 in a 28 d a y s b i o d e g r a d a t i o n test by f o l l o w i n g the DOC o f the c h e m i c a l in the i n c u b a t i o n flasks by colorimetric methods. 2 MATERIALS AND METHODS 2.1 Chemicals The following chemicals were tested. Standard compound Test compound: > C o m p o s i t i o n . Anil ine Purity. 99.5 X Fluorad FC-129 Potassium fluoro alkyl carboxylate Butyl jjiyCoT 50 V- 18 V. Uater 28 /. Ethanol 4% /V / Batch : 304 Uater solubility >2 g/1 at 25 d e g r e e s c e n t i g r a d e The t e 5 1 C h e m i c a l was s^upplied by 3f1 D e u t s c h l a n d GmbH, on J u l y 10, 1984. 2.2 Experimental design The s t u d y w a s run a c c o r d i n g to the OECD m e t h o d (1). 000373 RCC PROJECT 034244 FLUORAD FC-129 5 3 RESULTS 3.1 Degradation of test compound The r e s u l t s are p r e s e n t e d in S a m p l e F o r m S h e e t No 1 and F igure 1. 3.2 Degradation of standard compound (aniline) The re s u l t s are p r e s e n t e d in S a mple F o r m S h eet No 2 and F i g u r e 2. ^ CONCLUSION The t e s t c o m p o u n d , F l u o r a d FC-129, uias d e g r a d e d u n d e r the test c o n d i t i o n s uiithin 28 da y s to 90 7.. The s tandard, aniline, uras d e g r a d e d uthiri seven d a y s to 97 7.. The compound is considered to be readily degradeable. 5 REFERENCE OECD Guideline for teiVing of Chemicals-. 3 0 1 E: "R e a d y Biodegradability-. M o d i f i e d O E C D S c r e e n i n g T e s t " . f 000374 RCC PROJECT 034244 FLUORAD FC -129 SAMPLE FORM SHEET FOR THE MODIFIED OECD SCREENING TEST: NO 1 6 Date of sta r t of test: A u g u s t 17, 1984 Test/Standard material: Fluorad FC-129 Theoretical test cone.: 19.8 Inoculum: sec. effluent of a domestic sewage ( A R A - B i r s i g , T h e r w i l , CH) C a r b o n a n a l y s e r : T e c h n i c o n A u t o a n a l y s e r II, Method-No. 451-76 U mg C/l plant Jr , u V i,,ry> 3 r * L* f b Organic carbon content of test material 100 mg test material correspond t o : 13.5 mg organic carbon * Stock solution of the test material (734.5 m g / 1 0 0 ml, dilution 20 mi/1000 ml of nutrient solution) B: C a r b o n d e t e r m i n a t i o n s y Flask Culture m e d i u m No. Analyses Theor . cone mg/1 Q n oN-* DOC ** 7 after x days mg/i 14 21 27 28 Mineral nutrient solution with test material and with inoculum 1 al 19.8 a2 19.8 al +a2 ml 2 19.8 17.5 17.6 17.6 '3.3 3.6 4.1 4.1 #* 3.7 3.9 > 3.8 4.0 4.0 3.7 3.9 3.9 bl .19.8 17.7 fc 3.8 3.6 4.1 3.6 2 b2 19.8 17.7 *** 3 . 8 3 . 5 4.2 3.6 bl +b2 m2 a ---------- 2. Mineral nutrient solution without test material but with inoculum Blank cl c2' cl +c2 m 3 ------- 19.8 % - - 17.7 1.3 0.7 1.0 3.8 3.6 1.8 1.2 1.4 2.7 1 8 1.1 2.3 1.5 1.3 4.2 3.6 1.6 1.9 2.4 2.1 2.0 2.0 * Value determined with carbon analyser. ** All DOC values d e t e r m i n e d after c e ntrifugation. *** S a m p l e s lost d u r i n g a n a l y s i s . 000375 RCC PROJECT 034244 FLUORAD FCrl29 Sample form sheet_Hd . 1 cent. C . E v a l u a t i o n o f r a m data: 7 Flask No. V. D O C r e m o v a l after x days 7 14 21 27 28 DOC-concen trations minus blanks 1 ml t -m 3 1 Dl * 1 ........... . 100 *** 87 84 89 89 ml -m3 l v m 2 1 -m31 D2 - 1 ........... . 100 ### 36 86 87 90 m2 -m3 m e a n D = Dl D2 2 for day x *** 87 85 88 90 *** Samples lost during analysis. t 000376 RCC PROJECT 034244 ANILINE SAMPLE FORM SHEET FOR THE MODIFIED OECD SCREENING TEST: NO 2 6 Date of s t a r t of test-. A u g u s t 17, 1984 Test/Standard material-. Aniline Theoretical test cone.: 19.4 Inoculum-, sec. e f f l u e n t of a d o m e s t i c sewage ( A R A - B i r s i g , Th e r w i l , CH) C a r b o n a n a l y s e r : T e c h n i c o n A u t o a n a l y s e r II, Method-No. 451-76 U mg C/l plant A: O r g a n i c c a r b o n c o n t e n t of test mate r i a l : 1 0 0 mg test m a t e r i a l c o r r e s p o n d to-. 77.4 mg o r g a n i c c a r b o n * Stock s o l u t i o n of the test ma t e r i a l (25 mg/l> B -. C a r b o n d e t e r m i n a t i o n s -. Flask Culture m e d i u m No. Analyses Theor . DOC ** cone . mg/,1 0 <C0) 7 after x days mg/ 1 14 21 27 28 Mineral nutrient solution with test material and with inoculum 1' al 19.4 a2 19.4 al +a2 ml * ----- 19.4 -------- paw. bl 19.4 12.4 0 2.1 1.2 11.9 2.4 1.8 1.1 1.8 1.9 1.6 2.3 12.2 1.2 2.0 1.2 1.7 2.1 12.0 3.1 1.8 1.9 1.9 2.1 b2 19.4 10.9 2.7 1.6 1.4 1.8 2.1 Mineral nutrient solution without test material but with inoculum bl +b2 <ru:= 2 si' cl Blank c2 cl*c2 m 3 ----- L. .19.4 11 . 5 2.9 1.7 1.7 1.7 2.1 1.3 1.8 1.2 1.4 1.6 1.9 0.7 2.7 1.8 1.1 2.4 2.1 1.0 2.3 1.5 1.3 .0 * Value calculated. ** All DOC values d e t e r m i n e d after c e n t r i f u g a t i on 000377 RCC PROJECT 034244 ANILINE Sample form sheet. No. 2 cont. C: E v a l u a t i o n o f r a m data-. 9 Flask No. '/. D O C r e m o v a l a f t e r x days 7 14 21 27 28 DOC-concentrations minus blanks 1 2 mean D1 ml t-m31 1 ........... ml -m3 100 100 96 100 100 m 2 1 -m 3 1 D2 - 1 - - ....... ,. 100 94 98 m2 -m3 96 100 D* D1 + D2 97 97 98 100 for day x 99 99 99 3V- J*' t- 000378 000379 Figure 2: DOC-removal Test material: Aniline 000380 Sheetl ThOD of FC-129 *CM i $ 1) 50% FC SOLIDS: C8F17S02N(C2H5)CH2C00-K+ 11/91 NOTE: CARBON RATIOS ARE C4.C5.C6.C7.C8=2.5%.0.5i 2) 14% BUTYL CELLOSOLVE 3) 32% WATER 4) 4% ETHANOL FRACTION COMPONENTS 42.00% C8F17S02N(C2H5)CH2COO-K+ 2.00% C7F15S02N(C2H5)CH2C00-K+ 3.00% C6F13S02N(C2H5)CH2C00-K+ 0.50% C5F11S02N(C2H5)CH2C00-K+ 2.50% C4F9S02N(C2H5)CH2C00-K+ 14% C4H90CH2CH20CH2CH20H 4% CH3CH20H 32% WATER 100.00% TOTAL MW 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% 46 24 2.09% 18 0 0.00% 21.92% f . Page 1 000381