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Synthesis of IDAA silane. In a 1-L round bottomed flask, 30.5 mL (0.22 mol) of triethylamine was dissolved in 500 mL of dry tetrahydrofuran. The flask was then stoppered with a rubber septum and 24.4 mL (0.104 mol) of 3-aminopropyltriethoxysilane and 23.0 mL (0.208 mol) of ethyl bromoacetate (Caution! Lachrymator, were added sequentially via syringe. The mixture was stirred overnight under N2, then septum was removed and the flask fitted with a reflux condenser and mixture was heated to reflux for 5 h. At the end of this reflux period, it was cooled to room temperature and filtered to separate the precipitated Et3 N-HBr. The solvent was removed by distillation and the crude product subjected to vacuum distillation to afford 35.76 g (87.0 mmol; 84% yield) of a pale yellow liquid (bp 160-170 °C at 0.375 torr, 1H NMR (CDCl3) 4.15 (q, 4H, J, 7.2 Hz, 3.81 (q, 6H, J, 7.2 Hz, 3.55 (s, 4H, 2.71 (pt, 2H, J, 7.5 Hz, 1.59 (quintet, 2H, J, 8.1 Hz, 1.27 t, 6H
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3 N-HBr. The solvent was removed by distillation and the crude product subjected to vacuum distillation to afford 35.76 g (87.0 mmol; 84% yield) of a pale yellow liquid (bp 160-170 °C at 0.375 torr). 1H NMR (CDCl3) 4.15 (q, 4H, J = 7.2 Hz), 3.81 (q, 6H, J = 7.2 Hz), 3.55 (s, 4H), 2.71 (pt, 2H, J = 7.5 Hz), 1.59 (quintet, 2H, J = 8.1 Hz), 1.27 (t, 6H, J = 7.2 Hz), 1.22 (t, 9H, J = 7.0 Hz), and 0.61 (m, 2H). 13C NMR (CDCl3) 171.4, 60.4, 58.3, 57.3, 54.9, 21.2, 18.3, 14.2, and 7.6.
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Deposition into MCM-41. 10.017 g of MCM-41 (920 m2/g, 35 Å pores, 27,28] was suspended in 200 mL of toluene and treated with 3.2 mL of water to hydrate the silica surface [22, This slurry was stirred at room temperature overnight to insure uniform distribution of water throughout the sample. To this slurry, 11.0 g of the IDAA silane was added, and the mixture was heated to reflux for 4 h. After this reflux period, the reflux condenser was replaced with a short path distillation head and the ethanol and water azeotropes were removed via distillation. The product was then collected by vacuum filtration, washed copiously with 2-propanol and air-dried to give 13.752 g of a free-flowing white powder. Given that the original silica sample had a surface area of ∼9215 m2, and we observed a mass increase is 3.735g, if we assume a MW for the hydrolyzed silane of 267.05 g/mol (the HO-Si(O)-R assumption, see Ref, 19, this corresponds to approximatel
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2. For this silane, this corresponds to approximately 1.0 mmol/g.
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0012247651
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Beck J.S., Vartuli J.C., Roth W.J., Leonowicz M.E., Kresge C.T., Schmitt K.D., Chu C.T.-W., Olson D.H., Sheppard E.W., McCullen S.B., Higgins J.B., and Schlenker J.L. J. Am. Chem. Soc. 114 (1992) 10834-10842
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62649142003
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note
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3 solution to bleach out the color. At this point the sample was once again washed with water, and 2-propanol, then air-dried.
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31
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62649156944
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note
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f are the initial and final concentrations in the solution of the target species determined by ICP-MS, V is the solution volume in mL, and M is the mass in gram of the sorbent.
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34
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85047870218
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For an excellent summary of the structure and properties of activated carbons, see:, Taylor & Francis, New York pp. 1-51
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View Koonsiripaiboon, Vichaya Sukwarotwat, Jide Xu, Kenneth N
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Wassana Yantasee, Glen E. Fryxell, George A. Porter, Kanda Pattamakomsan, View Koonsiripaiboon, Vichaya Sukwarotwat, Jide Xu, Kenneth N. Raymond, Novel Sorbents for Removal of Gadolinium-based Contrast Agents in Sorbent Dialysis: A Preventive Approach to Nephrogenic Systemic Fibrosis (NSF) (submitted for publication).
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