High-performance Liquid Chromatographic Stationary Phases Based On Poly(methyloctylsiloxane) Immobilized On Silica I. Physical And Chemical Characterizations

Five different reversed-phase materials for high-performance liquid chromatography were obtained by deposition of poly(methyloctylsiloxane) in HPLC silica particles, followed by immobilization using different processes: thermal treatment (120 or 220°C for 4 h), irradiation with microwaves (495 W for 15 min), γ radiation (dose of 80 kGy) and self-immobilization. These phases were characterized by gel permeation chromatography, percent carbon, 13C and 29Si solid-state nuclear magnetic resonance spectroscopy, infrared spectroscopy, thermogravimetric analysis and scanning electron microscopy. The results show that the different immobilization processes produce different physical characteristics in the prepared phases. © 2002 Elsevier Science B.V. All rights reserved.9481-297107Vansant, E.F., Van Der Voort, D., Vrancken, C., (1995) Characterization and Chemical Modification of the Silica Surface, , Elsevier, New YorkPesek, J.J., Matyska, M.T., Sandoval, J.E., Williamsen, E.J., (1996) J. Liq. Chromatogr. Rel. Technol., 19, p. 2843Tani, K., Suzuki, Y., (1996) J. Liq. Chromatogr. Rel. Technol., 19, p. 3037Tani, K., Suzuki, Y., (1996) J. Chromatogr. A, 722, p. 129Sander, L.C., Wise, S.A., (1995) Anal. Chem., 67, p. 3284Sander, L.C., Pursch, M., Wise, S.A., (1999) Anal. Chem., 71, p. 4821Berthod, A., (1991) J. Chromatogr., 549, p. 1Nahum, A., Horváth, C., (1981) J. Chromatogr., 203, p. 53Sadek, P.C., Carr, P.W., Bowers, L.W., (1985) J. Liq. Chromatogr., 8, p. 2369Sadek, P.C., Koester, C.J., Bowers, L.D., (1987) J. Chromatogr. Sci., 25, p. 489Weber, S.G., Tramposh, W.G., (1983) Anal. Chem., 55, p. 1771Unger, K.K., (1979) Porous Silica: its Properties and Use as Support in Column Liquid Chromatography, , Elsevier, AmsterdamScott, R.P.W., (1993) Silica Gel and Bonded Phases: their Products, Properties and Use in Liquid Chromatography, , Wiley, ChichesterPoole, C.F., Poole, S.K., (1991) Chromatography Today, , Elsevier, AmsterdamOhtsu, Y., Shiojima, Y., Okumura, T., Koyama, J.I., Nakamura, N., Nakata, O., Kimata, K., Tanaka, N., (1989) J. Chromatogr., 481, p. 147Engelhardt, H., Löw, H., Eberhardt, W., Maub, W., (1989) Chromatographia, 27, p. 535Kirkland, J.J., Dilks, C.H.J., Henderson, J.E., (1993) LC-GC, 11, p. 290Wirth, M.J., Fatunmbi, H.O., (1992) Anal. Chem., 64, p. 2783Wirth, M.J., Fatunmbi, H.O., (1996) J. Liq. Chromatogr. Rel. Technol., 19, p. 2799Fairbank, R.W.P., Wirth, M.J., (1999) J. Chromatogr. A, 830, p. 285Akapo, S.O., Fatunmbi, H.O., (1999) LC-GC, 17, p. 334Schomburg, G., (1991) Trends Anal. Chem., 10, p. 163Schomburg, G., Deege, A., Köhler, J., Bien-Vogelsang, U., (1983) J. Chromatogr., 282, p. 27Bien-Vogelsang, U., Deege, A., Figge, H., Köhler, J., Schomburg, G., (1984) Chromatographia, 19, p. 170Hansen, M., Unger, K.K., (1992) Trends Anal. Chem., 11, p. 368Petro, M., Berek, D., (1993) Chromatographia, 37, p. 549Mao, Y., Fung, B.M., (1997) J. Chromatogr. A, 790, p. 9Nyholm, L.M., Markides, K.E., (1998) J. Chromatogr. A, 813, p. 11Figge, H., Deege, A., Köhler, J., Schomburg, G., (1986) J. Chromatogr., 351, p. 393Da Silva, M.C.H., Jardim, I.C.S.F., (1998) J. Liq. Chromatogr. Rel. Technol., 21, p. 2447Jardim, I.C.S.F., Collins, K.E., Anazawa, T.A., (1999) J. Chromatogr. A, 849, p. 299Collins, K.E., Bottoli, C.B.G., Bachmann, S., Vigna, C.R.M., Collins, C.H., Albert, K., Chem. Mater., , in pressCarraher, C.E.J., (1982) J. Macromol. Sci., A17, p. 1293Hetem, M.J.J., De Haan, J.W., Claessens, H.A., Cramers, C.A., (1991) J. Chromatogr., 540, p. 53Bachmann, S., Melo, L.F.C., Silva, R.B., Anazawa, T.A., Jardim, I.C.S.F., Collins, K.E., Collins, C.H., Albert, K., (2001) Chem. Mater., 13, p. 187