Document M43k94Dnwm85pYeOvE6O8nbRx

SOIL ADSORPTION (METHOD DEVELOPMENT / PILOT STUDIES) TEST SUBSTANCE_____________________________________________________ Identity: N-ethylperfluorooctane sulfonamidoethanol; may also be referred to as N-EtFOSE Alcohol or FM-3422. (1-Octanesulfonamlde, N-ethyl1,1,2I2,3,3,4,4,5I5,6I6 I7I7 >8,8,8-heptadecafluoro-N-(2-hydroxyethyl)-I CAS #1691-99-2) Remarks: Material is an off-white, waxy solid of uncharacterized purity. M E T H O D ______________________________________________________________ Method: The attached studies explore the use of organic solvents (1977 study) or Thin Layer Chromatography Plates (1978 study) for determining the soil mobility of N-EtFOSE alcohol. These methods were developed by 3M while looking for alternatives for studying the adsorption/desorption properties of the test substance. GLP (Y/N): No Year (study performed): 1977 and 1978 Statistical methods: None. Temperature: Not noted in the reports. Remarks field: Very little detail is available on these study methods. RESULTS______________________________________________________________ The 1977 study using 20% and 5% alcohol as a portion of the solvent indicated between 64% and 98% of the N-EtFOSE alcohol was sorbed to the sandy loam soil. The 1979 study using TLC greenhouse soil plates indicated that N-EtFOSE alcohol did not move from the spot it was placed. C O N C L U S IO N S ________________________________________________________ Both studies concluded that N-EtFOSE alcohol is likely to sorb to soil. Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 DATA QUALITY_________________________________________________________ Reliability: Klimisch ranking 3. These studies lack sufficient explanation of the methodologies. Purity of the test substance is not characterized. The analytical methodology is also either missing or lacks validation. REFERENCES______________________________ ___________________________ 006210 Method and results summary, "Adsorption of FM-3422 on Soil." Stephen K. Welsh, March 7,1977, April 12,1977, May 9, 1977. Excerpt from 3M Technical Notebood No. 48277 30, "Soil Thin-Layer Chromatography - FC 95, FC 143, FM 3422", Page 30, A. Mendel, Project Number 997061200, October 13, 1978 Review of Technical Notebook No. 48277-30. Soil Thin Layer Chromatography. Professor Stephen A. Boyd, Michigan State University, May 19,1993. OTHER Last changed: 5/18/00 006211 Attached are comments on the 3M Technical Report "Soil Thin Layer Chromatography - FC95, FC143, FM3422. A. Mendel, Project No. 997061200 3M Technical Notebook No. 48277, Page 30, Oct. 13, 1978 (one page from a technical notebook)" made by Professor Stephen A. Boyd, Michigan State University, dated May 19, 1993. 006212 Review of Technical Notebook No. 48277-30 Soil Thin Layer Chromatography I am not too sure how useful these plates are. Apparently both FC 143 and FM 3422 remained at the origin o f the thin layer plate where they were originally spotted. This implies no movement with the water used to develop the plate. Basically this tells me the method is insensitive, and doesn't yield much useful information. That is because FM 143 has a much lower soil sorption coefficient (K^ = 17) than FM 3422 (K^ = 15,000) and yet they behaved similarly in the soil thin layer chromatography plate. Mobility studies are probably best done in soil columns using micisible displacement experiments. These are more difficult to do experimentally but would yield more useful data that could be compared to other well studied compounds. The experimental approach is well established now and there are several laboratories doing this type of work, including my own. These experimetns augment batch equilibration (isotherm) experiments very nicely. 006213 JjE T N O . J 3 I . D ^ 'L b D a Subject: PAGE 3M TECHNICAL NOTEBOOK NO. 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R C_OH C E / v T R T I t a) F g H T T i v 0- < 1 >T a R. F. ~ B R mP Ll -- -- --------- -------------- --- - 1 ul< * h $ ' BrT COPY AVAILABLE 006214 Signature. 'Zci. c/Y u 'c^ i Read and Understood__ " ,. 006209 o a A - >3 g/_ Date:-- LL u iL p L V\ $ , \ + 3 6 % / e \W 7 */. ADSORPTION OH HM 37.22 (in FC-206) ON SOIL, 12/30/75 J . C tZ C I53 ^ /\0 O < ^ Soil - sandy loam, 40673, p. 17; air drie^ 1. Make up solutions of FC-206 in DI water at 600 ppm, 6,000 ppm, and 60,000 ppm. 2. In 500 ml flasks put 100g soil and 100 ml of the following solutions: Flask 18A - DI water Flask 18B - 600 ppm FC-206 Flask 18C - 6,000 ppm FC-206 Flask 18D - 60,000 ppm FC-206 3. Shake flask for 24 hours at 100 oscillation/minute. 4. Let soil settle and decant of the liquid. Centrifuge the liquid. RESULTS (12/30/75) FC-206 Cone. FM-3722 cone., ppm Equil. FM-3722 cone. C , ppm (measured) FM-3722 adsorbed, x/m, H8/g (calculated) % Adsorbed DI Water -- ... 600 ppm 4.2 0.14 4.1 98 6,000 ppm 42 2.2 40 95 60,000 ppm 420 210 210 50 Soil - sandy loam, 40673, p. 17; air dried Solvent - 20% alcohol in 1)1 water 1. Put a few mg FM 3422 (Lot 676) in the solvent and shake for at least 24 hours. Let FM 3422 settle and decant off the supernatant (the stock solution). 2. Make 10% and 1% dilutions of the.stock solution with'the same solvent. 3. Put 20g soil in each of 4-50 ml centrifuge tubes, then fill the tubes with DI water, shake thoroughly, and centrifuge five minutes at 6,000 rpm (4,000 G ) . 4. Pour off the water and add 20 ml of the sample solutions and 20 ml DI water in the blank. Shake the tubes for 24 hours (100-120 oscillation/min.). 5. After shaking, centrifuge as above and pour off the liquid. RESULTS (3/7/77) FM 3422 cone. ppm (measured) DI Water 23 /o#/,, 1.8 0.19 Equil. Cone. C , ppm (measured) -- 1.5 0.16 0.07 Adsorbed, x/m, pg/g (calculated) -- 21 1.6 0.12 % Adsorbed 9, 94 91 64 006215 ADSORPTION OF FM 3422 ON SOIL, 4/12/77 Soil - sandy loan, 40673,. p. 17; air dried Solvent - 5% alcohol in DI water 1. Put a few mg FM 3422 in the solvent and shake for at least 24 hours. Let FM 3422 settle and decant off the supernatant (the stock solution). Centrifuge at 10,000 rpm for 10 minutes. 2. Make 10% and 1% dilutions of the stock solution with the same solvent. 3. Put 20g soil in each of 4-50 ml. centrifuge tubes, then fill the tubes with DI water, shake thoroughly, and centrifuge at 10,000 rpm for 10 min. 4. Pour off the water and add 20 ml of the sample solutions and 20 ml DI water in the blank. Shake the tubes for 24 hours (100-120 oscillations/ min.). 5. After shaking, centrifuge as above and pour off the liquid. RESULTS (4/12/77) FM 3422 cone, ppm (measured) DI Water 44 3.9 0.5 Equil. cone. C, ppm (measured) --- 0.8 0.16 0.08 Adsorbed x/m, pg/g (calculated) -- 43 3.7 0.42 % Adsorbed -- 98 96 4 ADSORPTION OF FM 3422 ON SOIL, S/9/77 Soil - sandy loam, 40673`, p. 17; air dried Solvent - 5% alcohol in DI water * iV . '1 ?. 1. Dissolve 50.0 mg FM 3422 (Lot 676) in 50,0 ml alcohol. Put this solution into a one liter volumetric and maike up to mark with DI water. 2. Let the above "emulsion" stand for five days. (A white floe appeared in the bottom) Centrifuge some of.the supernatant at 10,000 rpm for 10 min. 3. Make 75%, 50%, 25%, and 10% dilutions of the stock solution with the same solvent. 4. Put 20g soil in each of 6-50 ml centrifuge tubes, then fill the tubes with the 5% alcohol solvent, shake thoroughly, and centrifuge five minutes at 5;000 rpm. 5. Pour off the solvent and add 20 ml of the sample solutions and 20 ml DI water in the blank. Shake the tubes for 24 hours (100-120 oscillations/ min.) b. After shaking, centrifuge (5,000 rpm, 5 min.) and pour off the liquid. RESULTS (5/9/77) FM 3422 cone., ppm (measured) DI Water 3.1 2.25 1.5 0.64 0.38 Equil. cone., C, ppm (measured) --- 0.06 0.05 * 0.02 0.02 Adsorbed, x/m, pg/g (calculated) -- 3.0 2.2 * 0.62 0.36 % Adsorbed* 98 98 * 97 9S 0 0 6 2 i * Dropped the sample