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Russ.Chem.Bull., Int.Ed., Vol. 56, No. 11, November, 2007
Klement´eva et al.
the ampule was sealed and heated for 4 h at 350 °С. Volatile
products, being a colorless transparent liquid, were frozen into a
trap and then analyzed by the LCꢀMS method. At this step the
amino groups were eliminated as organic amines with methyl
and propyl substituents. The thermal condensation of polymer
molecules gave TMP, APTES, and its liquid analogs. The conꢀ
tent of these compounds in the distilledꢀoff liquid was low and
totally at most 5—10%. Amines, TMP, and APTES were identiꢀ
fied by the mass spectra available from the data base. In addiꢀ
tion, the chromatogram contained two peaks, whose retention
times were higher than that for APTES. As a whole, the mass
spectra of these compounds differ slightly from the spectrum
of APTES and contained the ions characteristic of APTES.
Therefore, we assumed that these substances were 3ꢀ(methylꢀ
amino)propyltriethoxysilane and 3ꢀ(dimethylamino)propylꢀ
triethoxysilane.
9. M. Nogami, Y. Daiko, Y. Goto, Y. Usui, and T. Kasuga,
J. SolꢀGel Sci. Technol., 2003, 26, 1041.
10. M. Nogami, K. Miyamura, Y. Kawasaki, and Y. Abe,
J. NonꢀCryst. Solids, 1997, 211, 208.
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13. A. E. Mal´shikov, Zh. Neorg. Khim., 1987, 32, 2370 [J. Inorg.
Chem. USSR, 1987, 32, 1383 (Engl. Transl.)].
14. H. Mayer, Monatsh. Chem., 1974, 105, 46.
15. C. J. Brinker and G. W. Schere, SolꢀGel Science: The Physics
and Chemistry of SolꢀGel Processing, Academic Press,
Boston, 1990.
16. Ph. Massiot, M. A. Centeno, I. Carrizosa, and J. A.
Odriozola, J. NonꢀCryst. Solids, 2001, 292, 158.
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N. J. Clayden, E. Marenna, and E. Fanelli, Chem. Mater.,
2005, 17, 2081.
18. M. G. Voronkov, E. A. Maletina, and V. K. Roman,
Kremnekislorodnye soedineniya nemetallov. Proizvodnye azota
i fosfora [SiliconꢀOxygen Compounds of Nonmetals], Nauka,
Novosibirsk, 1988, 365 pp. (in Russian).
B. Weighed samples (0.1—0.2 g) of the powder calcined at
350 °С in quartz ampules 7×100 mm in size were placed in broad
vertical quartz tube and left in air under atmospheric pressure or
were blown with oxygen or argon. Then the ampules were heated
in an electric oven to 600 or 1000 °С, stored for 5 h, and cooled
to ~20 °C.
19. S. N. Borisov, M. G. Voronkov, and E. Ya. Lukevits,
Kremneorganicheskie proizvodnye fosfora i sery [Organosilicon
Derivatives of Phosphorus and Sulfur], Khimiya, Leningrad,
1968, 292 pp. (in Russian).
This work was financially supported by the INTAS
Foundation (Grant 03ꢀ51ꢀ5959), the Russian Foundaꢀ
tion for Basic Research (Project Nos 05ꢀ03ꢀ32556, 06ꢀ
03ꢀ81005 Bel, and 06ꢀ03ꢀ08208), the Council on Grants
at the President of the Russian Federation (Program for
State Support of Leading Scientific Schools, Grant
NSh 8017.2006.3), and the Presidium of the Russian
Academy of Sciences (Complex Programs "Fundamental
Problems of Physics and Chemistry of Nanosized Sysꢀ
tems and Nanomaterials" and "Target Synthesis of Subꢀ
stances with Specified Properties and Creation of Related
Functional Materials").
20. J. Livage, P. Barboux, M. T. Vandenborre, C. Schmutz, and
F. Taulelle, J. NonꢀCryst. Solids, 1992, 147—148, 18.
21. E. Pretsch, T. Clerc, J. Seibl, and K. Biemann, Tables of
Spectral Data for Structure Determination of Organic Comꢀ
pounds, SpringerꢀVerlag, Berlin—Heidelberg, 1989.
22. Yu. Yu. Samitov and T. V. Zykova, in Trudy tret´ei
konferentsii "Khimiya i primenenie fosfororganicheskikh
soedinenii" [Works of the Third Conference "Chemistry
and Application of Organophosphorus Compounds"], Nauka,
Moscow, 1972, 49 (in Russian).
23. Phosphorus. An Outline of its Chemistry, Biochemistry and
Technology, 2nd ed., Elsevier, Amsterdam—Oxford—New
York, 1980.
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Received January 29, 2007;
in revised form August 21, 2007