Document zoJbwpJMnQRjL43E4Z7evLa43

SOIL ADSORPTION (METHOD DEVELOPMENT /PILOT STUDIES) TEST SUBSTANCE Identity:N-ethylperfluorooctasnuelfonamidoethanolm;ay alsobe referredto as N-ETFOSE Alcoholor FM-3422. (1-Octanesulfonamide,N-ethyl1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluoro-N-(2-hydroxyethyly, CAS # 1691-99-2) Remarks: Materialisan off-whitew,axy solidofuncharactedzed purity. METHOD Method: The attachedstudiesexplorethe use oforganicsolvents(1977 study)orThin Layer Chromatography Plates(1978 study)for determiningthe soilmobilityofN-ETFOSE alcohol.These methods were developed by 3M whilelookingforaltemabves forstudying the adsorption/desorptiopnropertiesofthe testsubstance. G LP (YIN): No Year (studyperformed):1977 and 1978 Statisticmaelthods: None. Temperature:Not notedinthereports. Remarks field: Verylittdleetaiilsavailabloen thesestudymethods. RESULTS The 1977 study using20% and 5% alcoholas a portionofthe solventindicated between 64% and 98% ofthe N-ETFOSE alcoholwas sorbed tothesandy loam soil.The 1979 studyusingTLC greenhouse soilplatesindicatedthatN-ETFOSE alcoholdidnot move from the spot itwas placed. CONCLUSIONS Both studiesconcluded thatN-ETFOSE alcoholislikeltyo sorbtosoil. Submifter: 3M Company, EnvironmentalLaboratory,P.O. Box 33331, St.Paul, Minnesota,55133 DATA QUALITY Reliability:Klimischranking3. These studieslacksufficienetxplanationofthe methodologies. Purityofthetestsubstance isnot characterizedT.he analytical methodology isalsoeithermissingorlacksvalidation. REFERENCES Method and resultsummary, "AdsorptionofFM-3422 on Soil."Stephen K. Welsh, March 7, 1977, April12,1977, May 9, 1977. Excerptfrom 3M TechnicalNotebood No. 48277 30, "SoilThin-Layer Chromatography - FC 95, FC 143, FM 3422",Page 30,A. Mendel, Project Number 997061200, October 13,1978 Review ofTechnicalNotebook No. 48277-30. SoilThin Layer Chromatography. ProfessorStephen A. Boyd, Michigan StateUniversityM,ay 19, 1993. OTHER Last changed: 5/18/00 Attachedareconunentson the3M TechnicalReport "SoflThin Layer Chromatography - FC95, FC143, FM3422. A. Mendel,ProjectNo. 997061200 3M TechnicalNotebook No. 48277,Page 30,Oct. 13,1978 (one page from a technicanlotebook)"made by ProfessorStephenA. Boyd, Michigan StateUniversityd,atedMay 19,1993. Review of TechnicalNotebook No. 48277-30 SoilThin Layer Chromatography I am not too surehow usefultheseplatesare. Apparentlyboth FC 143 and FM 3422 remained at the originof the thinlayer'platwehere theywere originallsypotted.This impliesno movement with the water used to developthe plate. Basicallythistellsme the method is insensitivea,nd doesn'tyieldmuch usefulinformation.That isbecauseFM 143 has a much lower soilsorptioncoefficie(nKt,,=, 17)thanFM 3422 (K,,,= 15,000)and yettheybehaved similarliyn thesoilthinlayerchromatographyplate. Mobilitystudiesare probablybest done in soilcolumns using micisibledisplacement experiments.These are more difficulttodo experimentallbyut would yieldmore usefuldata thatcould be compared to otherwellstudiedcompounds. The experimentalapproachiswell establishendow and thereare severallaboratoriedsoing thistypeof work, includingmy own. These experimetriasugment batchequilibratio(nisotherm)experimentsvery nicely. 'JECT No. -9ti7 U L-Y ;ubicct: S n IL -r ti Object: T-Z R-MFRT Reference: t t h h N - 3M TECHNICAL NOTEBOOK NO. Date: PAGE 4BZ717 *to 1 C3- 1-9--7B T-P=, L 4 R ElM P Ta S M q P Rt -OL14 s e@ FC Ili FM 3-A ZZ- = 7! 1 r.: -------.-* 1-7) rmUILS =C3UN-5 C-MPIR%C-AI-L@t Tt4Rr rf4E aist3 Mir-kMtJ Ett'Lf r.3EllL Ff%wr%c-(aS 5 LtJR'kkr--7LnIC)-0r W 14TE- P% FKNM C-tltRTr-1-3 CaN Ezt-tl@nri -t3LRTr--s rjfqVF- rclya-aCIVC-P,.PLL- 13LIATIE%_-,.rALtri%l:t%.twi@L-Yriie-Pmi-t-mwotiE. ujf4l:3-Gtlue-. iqkj Ai-rimsrt---MiyrLiRF_ 13r- ISC].g. oF: 25-13 rnir a ti (EVr-@a a P.C-Eiv - 14MU'SE SMTL- ENRT-RIOED FRt3M L4. SEt-46 lS6,1%Lt-kEM p"-a %CJIL at]!Vt-:13*JayM.T.I! S#J'o 1-.H. Pt"ztrl.@i-kF;It@FjIN13 E3[1 ML. ujprr--rk Luf4S WP-Lt--""444(RK.C-,FA:/;?J"BISPRE14M 13OTra TC- iJ io @&2-(3r-M . r7LR Sri 'PLfqTr@.L-iCijEir uji4rc-R TCS MRKE rniili-wFZe-@3o Gr#4ILy LF-Sr. V ir:3LDJ S rim F-:-rP,%f ur=t toir. 8 S -9(1 ML. A m -a Fi-fStf3 rAC-RD IK)ro rn Ft-yiar- r31-iGptk-TL-i aLs ticK@e- F:z 1-14E-.P Lfk r E S ul (qt-Liw r--D r El F;'P, 13 R Y. T 0 F- r4,PR C-F-*M E P. Li S V--T:S-rn r-Cl RT rtif flc-Flr a j@3 t.U9 S '0 E. '*t'&N -E713 t-lY -33R'. 3-.ui r-U- S LE E;, r=UT14 P, iT-z rnAr-t4 1v E &.a C,Nr-- oF tlII r4fv-a _r tqr__ 10 Y-013 r-M kmF LIFLF4 -r-F13 L4!(4 IJUTrt3t-nwlt+ Rqmtu L-si3F-Lr--U r-C 95 (&-C-r-r r+r3.ENE VtC-U_15Pt.FlTe-) *,r3POrS LUERE 0 *rT-V.'I] r-M i=Fkima rf4E @iulUULX--)Ffivl(a--M @3'42a -@d SPPL@(ED t3y r-O(VNtE'SR-HFZRI7Vn-r.Tt+r- Pf-"T F kx,n 1! -ur-IjL;-L-ti%-rJ--M IC CS rrtM. IAi F* r-ILRF-R FL14 Vk T, W (4f;-rM F4 E ts1;,roR virI Lj pk I U 14 1r(4 44 (=rtr TK E -aiFvLr---" P M E W'r A e MU (K Lric) lllatOlT- 1 14p, +ClM I f4t P &_F4rF LljF4ra F; I1:@13 Rt E: 13 -r Lo f?si tvara T3 rwtq 7- ulhev rl4 E ,eat -t TL@r- P i-14TF_ W A 5 ilL-42.@EU (Ni-a -riiF- 7 ftN K J@-CINT-RIAJ(IVD A aL Li-r i T-(TI13 e t P tA (4rE. R 'T#4F- 13(L- ifirt4 F- w qrr--K r4Rq M Wlq LL-Y r-ELL_.FR U M 'rt4r- P LJIT r- aijt 'rijira 1017L Ivi)I- a F-p-r( r 13 114FFF-1-T PilEILE@35. .4 1 -Z Llir -r13 1-7-r- L))F(!5 T13 F fkImr F:0. p, v IS tjA L. ir-FirlisA;. -T14i=_ L-%ILd p,14iclIliR r--trv f-ry 15f;m T14 P- iCoMpIL%-% mmlr5 ?,,Iq:u-itt E. 01 6tkv=-R r_no r-E:t%irfFq:0%''9r1fA) nF r-JIL.UT-TtI--I(eJI@ 1-n(3OLfe- VkMP Ll-=) 7,r Signature Re:i(;iin(Liln(lcr%tood Date: S7 It 3 C.) c.- AL).SOIUITIOOllq.-I:M37.22 (in FC-206) 014 SOIL, 12/30/75 Soil - sandy loam, 40673, p. 17; air driecl 1. ,takeup solutions of FC-206 in DI water at 600 ppm, 6,000 ppm, and 60,000 PPM2. 111 500 ml flasks put lOOg soil and 100 ml of the following solutions-. I:Iask 18A Di water I-'Iask18B 600 ppm FC-206 I:lask 18C 6,000 ppm I:C-206 I:lask 18D 60,000 ppm FC-206 3. Shake flask for 24 hours at loo oscillation/minute. 4. Let soil settle and decint of the liquid. Centrifuge the liquid. RESULTS (12/30/7S) 1:(:-206Cone. 1:!4-3722conc., ppm Equil. 1,'M-3722conc. C, ppin (measured) I-'NI-3722Ldsoi-bed,x/m, pg/g (calculated) Adsorbed 01 Water ----- --- 600 ppm 4.2 0.14 4.1 98 6,000 ppm 42 2.2 40 gs@ 60,000 ppm 420 210 210 so ADSORI"R iON 0 SO I1., 3/ 7 7 7 Soil - sandy loam, 40673, p. 17; air dried Solvent - 20% alcohol in I)lwater 1. Put a few mg I-M 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. f4ake10% and 1% dilutions of tht.stock solution with the same solvent. 3. Ilut20g 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/win.). S. After shaking, centrifuge as above and pour off the liquid. RESULTS (3/7/77) a oV, FM 3422 conc. ppm (measured) Di Water 23 too/IV 1.8 1% 0.19 Equil. Conc. C. ppm (measured) 1.5 0.16 0.07 Adsorbed, X/m, pg/g (calculated) 21 1.6 0.12 t Adsorbed 94 91 64 ADSORPTION-OF FM 3422 ON SOIL, 4/12/77 Soil sandy loan, 40673,.p. 17; air dried Solvent - 5% alcohol in DI water 6 I . l'uta few mg FM 3422 in the solvent and shake for at least 24 hours. Let I:M3422 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. [our 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.). S. After shaking, centrifuge as above and pour off the liquid. RESULTS (4/12/77) FM 3422 conc. ppm (measured) Equil. conc. C, ppm (measured) DI Water Adsorbed x/m, pg/g (calculated) % Adsorbed --- 44 0.8 43 98 3.9 0.16 3.7 96 0.5 0.08 0.42 84 ADSORPTION OF FM 3422 ON SOIL, S/9/77 Soil - sandy loam, 4067r,-p. 17; air dried Solvent - 5% alcohol in Di water 1. Dissolve 50.0 mg FM 3422 (Lot 676)..in50.0 ml alcohol. Put this solution into a one liter volumetric and make ul)to mark with DI water. 2. Let tticabove "emulsion" stand for five days. (A white floc appeared in the b.ottom) Centrifuge some of.the supernatant at 10,000 rpm for 10 min. 3. Make 75%, 50%, 2S%, and 10% dilutions of the stock solution with the s solvent. 4. I)ut20g soil in each of 6-SO ml centrifuge tubes, then fill the tubes with the S% alcohol solvent, sliakethoroughly, and centrifuge five minutes at 5 '000 rpm. S. P;ur 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.) 6. After sliaking,centrifuge (S,000 rpm, 5 min.) and pour off the liquid. RESULTS (5/9/77) Ft-I3422 conc., ppm (measured) DI Water 3.1 2.2S 1.5 0.64 0.38 Equil. conc., C, ppm (measured) Adsorbed, x/m, pg/g (calculated) --- Adsorbed 0.06 3.0 98 O.OS 2.2 98 0.02 0.62 97 0.02 0.36 9s Dropped the sample Fn For=474'?-II-A TECHNICAL REPORT SUMMARY TO: TECHNICAL COMMUNICATIONS CENTER - 201-2CN (importont- Ifreportisprintedon boM sidesofpVw, ondtm copiesm TCC.) Division Environmental Laboratory (BE IgPC). Project Report Title Fate of Fluarochemicals Analytical Methodology To D. L. Bacon Author(s) Arthur Mendel Noubook R*Iorence .41947, 44191, 46269, and--Sui:)port 47703, 48277, 49400 SECURITY C)open tcompow Confkbntw) 11 Closed ISpeciaAluthorintion) 3M CHEMICAL REGISTRY KEYWORDS: (Selwtwrm fmm 3M Thowuna. Suosa atmr awlicableterm&) CURRENT OBJECTIVE: Progre-,-s Report EE & PC-Div. Fluorochemicals 1/17/79 Dopt Number - .0535 Project Nurnbw 9970612643 RePort Hurnbw .008 Employee Number(sl 043939 t4o.-oT?r"" .eluding Covorohmt 22 Now Chwni=ls Reported C) Yes M No REPORT ABSTRACT-. (200-2SO words) This abstractlnfam-ation isdistributebdy theTochnkal Communimtsons alert3M'ers to CnnV&ny R&D. It isCompany confidential material. Centetro Information Liaison lnitiwc 3PACONFIDENTIAL FM 3422 Sorption ()ntoSoil (46269-50) Sorption-desorption soil studies were conducted by S. K. Welsh, and the results are given in Table 2. Soil TLC (48277-30) Various types of soil were ground and sievedand that fraction of 262 micron size was saved for TLC studies (42669-42). An intimate mixture of 150 g of 262 micron size greenhouse soil (sandy loam) with 80 ml of water was well slurried and spread onto 10 x 20 em glass plates using an in-house designed spreader (designed by J. W. Belisle, A. Mendel, and G. Guthrie). The plates were allowed to air dry. A plate was spotted 2 em from the bottom with radiolabeled-FC-95,-FC-143, and-FM*3422. The samples were those used earlier for water solubility studies. The plate was air-dried and developed 100 mm from the original spot in the ascending mode with water in a filter paper-lined TLC developing tank previously equilibrated with water for one day. The development required nearly two hours and the air-dried plate was then autoradi ()graphed (13). results -;howed tliit FC-143 and FM 3422 did not leave the origin (R =0). The spot, due to FC-95, was extremely laint for visualizatisn but appears not-to have migrated either (R =0). f Preliminary Studies on Samples from Bionomics Labs A. Examination of Foil-lined Caps for Interferences (46269-50) Four foil-lined caps which Bionomics Labs uses to seal bottles containing samples were screwed onto four clean bottles containing 25 ml of deionized water. The bottles were mechanically shaken for 4 hours,and the combinea .100 ml of water was extracted with ethyl acetate. This extract was concentrated and chromatographed. No apparent interference for FM 3422 was noted. This extract was then spiked with FM 3422 to confirm no interference at the retention time of FM 3422. B.. Examination oC Standards and Controls Prepared at Bionomics Lab Personnel from Bionomics Labs prepared standard solutions of FM 3422 in water, then submitted one-liter samples of these standards and controls to us for analyses. The respective sample was extracted with ethyl acetate and the organic extract was concentrated to 10 ml. An aliquot was used then for GC analyses, and the results are summarized in Table 3 (Notebook 46269-50). Table 3 Analyses for FM 3422 (in ppb) in Bionomics Samples Sample I.D. A5609 A5610 A5611 A5612 A5613 A5614 A5615 A5616 A5617 Theoretical Conc. (ppb) 20 20 10 10 5 5 2.5 2.5 1.25 Determined 20.8; 19.8 19.8; 20.6 10.2; 9.9 9.7; 10.1 5.2; 5.2 4.8; 5.1 2.5;,2.6 1.2; 1.3 (a) A5618 1.25 (a) A5619 A5620 A5621 Control A Control B Solvent Control A <0.1 <0.1 <0.1 A5622 Solvent Control B <0.1 A5670 A5670 1.25 1.25 1.1; 1.0(b) 1.0; 1.6(b) (a) received broken in shipment; (b) replaces original samples A5617; A5618