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N-ETFO WATER SOLUBILITY TEST SUBSTANCE Identity:N-ethylperfluorooctasnuelfonamidoethanolm;ay also be referredto as N-ETFOSE Alcoholor FM-3422. (I-Octanesulfonamide,N-ethyl1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluoro-N-(2-hydroxyethyl)-, CAS # 1691-99-2) Remarks: Materialisan off-whitew,axy solidofuncharactedzed purity. METHOD: Method followed: The Vefth-Comstock technique,G. D. Veithand V. M. Comstock, J.FishRes. Board Can.,32,1849 (1975) GLP: No Year study was performed: 1977 Remarks: This experiment was performed 8 times. No informationisgiven on sample purity. RESULTS Value (mg/L) at20 C: Mean value 0.05(0.04-0.062Range over8 trials) CONCLUSIONS The testsubstance has solubilitiynthe mid partper billiornange. DATA QUALITY ReliabilityK:limischranking= 3. Itisusefulinthatitindicatesthe approximate N-ETFOSE alcoholwater solubilityT.he testwater was not sufficiently characterized,norwas the purityofthe testmaterialnoted. Testingwillbe redone using currentmethods and analyticatlechniques.Testing willbe conducted using a purifiesdample. REFERENCES 3M TechnicalReport Summary, Fate of Fluoroche'micals3,M Environmental Laboratory,3M EnvironmentalEngineeringand PollutionControl,A. Mendel, 11/15/77 OTHER Submitter: 3M Company, EnvironmentalLaboratory,P.O. Box 33331, St.Paul, Minnesota,55133 Last changed: 5/18/00 .4 3m For=47-11 A TECHNICAL REPORT SUMMARY ,Y: TECHNICAL COMMUNICATIONS CENTER 201-2CN (Important- ifreportisprintedon bo0 sideosfpaper,m7d t" copiestoTCC.) Division Proiect Report Title To Authorls) Notebook Roforerbco Environmental Laboratory (EE_& PC) Fate of Fluorochemicals Analytical Methodology on FM 3422 D. L. Bacon A. Mendel SECUR ITY open Cloud (Company Confidential) (SpeciaAluthorization$ KEVWGRDS: IS*Ioctermsfrom 3M ThesaurusS.ugpst other applicablteorms.i CURRENT OBACTIVE, 3PACHEMICAL REGISTRV HE & PC-Div. Fluorochemical Analytical Progress Report Date 11/15/77 Dept. Number 0222 Project N um bar 9970612643 Report Number rr-nplov" Number(s) 43939 -No. of Pages Including Coverihoot 13 Now ChwnWo Reported 0 Yet FL)No REPC)RTABSTRACT:(200-2w5or0ds) This abstraicntformatiisdoinstribbuyttehdeTechnicCaolmmunicaticoennstetro star3tW*rstoCompanRy&D.ItisCompanyconfidenmtaitaelrial. lnfotmation Liaison -9- UETERMINATION OF SOLUBILITY OF FM 3422 IN WATER The Veith-Comstock technique (2) was used for this experiment. Glass beads (ca. 300 g, 3 ma. in diameter) were added to a solution of 100 mg of FM 3T22 in about 500 ml of acetone. ihe solvent was allowed to evaporate, thus depositing the fluorochemical on the beads. The beads were packed into a colunn (ca. 25 mm. dia. x 4SO mm.) whose end was prepacked with a 20 mm. layer of silanized glass wool, followed by a 20 mm. layer of sand. The top of the co packed with a 20 mm. layer of silanized glass wool, was attached by Mayon timt ubing to the top inlet of a 2-liter bottle filled with water. The bottom of the column was attached by tubing through a peristaltic pump, to the bottom outlet of the 2-liter flask. The water was circulated upwards by the pump through the column for about two weeks. By volumetric pipet, one hundred milliliters of satu'rated liquid was withdrawn, diluted with 10 ml of aqueous saturated salt, and extracted 3 times with a total of 21 ml of ethyl acetate. The combined extract was diluted to 2S al (volumetric flask). An aliquot was gas-chromatographed. This experiment was performed eight times. The results are reported in TABLE III. TABLE III SOLUBILITY OF FM 3422 IN WATER* Experiment No. ppm FM 3422 1 2 3 4 5 6 7 Mean *Temp. Mean 0 20 c . 0.05 ppm; Range .0.050 0.045 0.061 0.042 0.040 0.062 0.050 0.048 0.04975 0.04-0.062 ppm; Std. Dev. 0.0084 RI:COVERY STUDIES OF AQUEOUS FM 3422 SOLUTIONS IN VARIOUS CONTAINERS (44191-42) At the low solubility level of FM 3422 in water (0.05 ppm), the possibility was considered of incomplete recoveries due to sorption of FM 3422 by plastics and/ or glass. Accordingly, the following study was made: -10- Revised 12/27/77 One hundred milliliters on 0.05 ppm FM 3422 in water (by the Veith-Comstock technique (2) as described earlier) was added to an amber glass - and to a polyeihylene - container, respectively. The containers were capped and allowed to stand in the laboratory for one week. The respective contents of the containers were transferred quantitatively to a separatory funnel. The container was.rinsed with two milliliters of water only. To the funnel was added 10 ml of saturated aqueous sodium chloride and 19 al of ethyl acetate. The contents were extracted and the organic extract was transferred quantitatively to a 25 ml volumetric flask. The aqueous phase was re-extracted twice with 5 ml of ethyl acetate. The combined organic extract was diluted to the mark (ethyl acetate) and then gas chromatographed. To each of the now empty containers used above was added (pipet) 1 ml of methanol. The respective container was sealed, rinsed with this 1 ml of,methanol, and an aliquot was gas chromatographed. Experiments were performed in duplicate and the results are indicated in TABLE IV. TABLE IV CONTAINER STUDIES WITH FM 3422 Experiment No. Container PM 3422 in 100 ml water (lig) Total FM 3422 in Container: Methanol Rinse (ug) Total FM 3422 Recovered* (iig) 1 Glass 5.8 2 Class 4.6 3 Polyethylene <3 4 Polyethylene <3 0.04 .0.19 1.88 1.15 5.8 4.8 <4.9 <41.-2 *Solubility of FM 3422 in water determined as 0.05 ppm or 5 ug/100 ml. It appears therefore that glass containers may be used but polyethylene must riotbe used to store solutions at these concentrations; otherwise, severe losses of material are possible.