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  • 1
    ISSN: 1435-1536
    Keywords: Key words Time-resolved near-infrared ; Two-dimensional correlation ; 3-Aminopropyltriethoxysilane ; Condensation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract The polymerization behavior of 3-aminopropyltriethoxysilane, a process initiated by water molecules, has been examined using time-resolved near-IR and 2D near-IR correlation spectra. By deconvolution of the time-resolved near-IR spectra, the existence of the component bands at 5189, 5265 and 5300 cm−1, whose intensities decrease markedly as the reaction proceeds, has been confirmed in the 5000–5400 cm−1 region. The band at 5189 cm−1 has been assigned to water molecules, while those at 5265 and 5300 cm−1 have been assigned to the strongly and weakly associated silanol groups, respectively. The kinetics of the hydrolysis of the ethoxy groups and of the formation of a siloxane bond have been analyzed using the time-dependent integral intensities of these three bands and the mechanisms of the reactions have been discussed. Evidence for this polymerization process is also clearly evident in the 2D near-IR correlation spectra.
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  • 2
    ISSN: 1435-1536
    Keywords: Key words Perfluorooctyl-trimethoxysilane ; Mass fractal ; Small-angle X-ray scattering
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract The acid-catalyzed condensation reaction of perfluorooctyltrimethoxysilane (PFOS) and n-octyltrimethoxysilane (OTMS) in ethanol has been followed by time-resolved synchrotron radiation small-angle X-ray scattering (SAXS) on a short time scale. SAXS curves for PFOS and OTMS have been interpreted as arising from mass fractals with D f=2 (PFOS) and D f=1.7 (OTMS). The time dependence of the apparent radius of gyration, obtained from the Guinier plots, showed that the growth of fractal precursors occurs in a two-step process within 2 h for PFOS and within 1.5 h for OTMS, in which small clusters involving monomers, dimers and trimers are formed in the initial step and formation of larger clusters occurs in the second step. Furthermore, it has been suggested that the hydrophobicity and lipophobicity of the bulky alkyl groups may also contribute to the formation of these giant aggregates.
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  • 3
    ISSN: 1435-1536
    Keywords: Key words 3-Aminopropyltriethoxy-silane ; CMC ; reversed micelles
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract  Changes in the 13C and 1H NMR chemical shifts of the silane coupling agent (3-aminopropyltri-ethoxysilane, APTS) in toluene, which were detected as the concentration of APTS increased, have been interpreted in terms of the formation of micelles and the presence of a critical micelle concentration (CMC) equal to ca. 0.47 mol 1-1. For the protons of the n-propyl segment, 1H NMR splitting patterns have been analyzed and conformations of the propyl segment have been discussed. Plots of relative absorbance of the two NH2 stretch IR bands at 3324 and 3384 cm-1 against concentration provided an inflection point (corresponding to the CMC) at a value equal to 0.46 mol 1-1. Thus, consideration of the interaction of APTS with a surface must take into account the presence of both APTS aggregates as well as APTS monomers.
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  • 4
    ISSN: 1435-1536
    Keywords: Key words Raman ; polyamino-propylsiloxane ; GABA ; CH2 rock and skeletal stretch
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract  The Raman scattering spectra for polyaminopropylsiloxane (poly-APS) samples in the solid state and in aqueous solution and for the related compounds, γ-aminobutyric acid (GABA) and its hydrochloride salt (GABA ⋅ HCl), have been examined in the CH2 rock and skeletal stretch region. The Raman spectrum of the solid poly-APS sample may be accounted for by direct combination of the Raman spectra for GABA and GABA ⋅ HCl, whose crystal structures have been elucidated by a single-crystal X-ray diffraction study, suggesting that the APS segments of poly-APS in the solid state are in a conformationally ordered state. It has also been found that the Raman spectra of the solid and aqueous poly-APS samples in this region are useful for diagnosing the conformations of APS moieties bound onto the surface of silica gel.
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  • 5
    ISSN: 1435-1536
    Keywords: Key words 3-aminopropyltriethoxy silane ; silica gel ; interaction ; kinetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract  Three silica gel sample systems, modified with 3-amino-propyltriethoxy silane (APTS), were prepared by sequentially sampling the reaction mixture at various time intervals. The concentrations of 3-aminopropylsilyl groups (APS) bound on the silica surface were determined by elemental analysis. For the same sample systems, 29Si NMR intensities of an (–O)4Si species belonging only to the silica gel particles and corrected by a cross-polarization correction factor were also measured. Both the APS-concentrations and the correc-ted 29Si NMR intensities depended upon reaction time, reflecting the rate of the APTS–silica gel reaction. Kinetic analysis of these data was made by use of the Gauss–Newton method, and the overall reaction was found to consist of three reaction processes (an initial fast reaction, a slower second reaction and a much slower third reaction). In particular, the conversion of (–O)3SiOH to (–O)4Si is predominant in the second reaction process and the pore size of a silica gel particle affects the reaction mechanism.
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  • 6
    ISSN: 1435-1536
    Keywords: Key words DRIFT ; APTS ; silica gel ; NH2 behavior
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract  Three silica gel sample systems, modified with 3-amino-propyltriethoxysilane (APTS), were prepared by sequentially sampling the reaction mixture at various time intervals, and the diffuse reflectance infrared Fourier transform (DRIFT) spectra of these samples were measured in the regions 2700–3500 and 1300–2000 cm-1. The IR bands observed at 1597 and 1629–1633 cm-1 were assigned to the deformation modes of NH2 and NH+ 3 groups, respectively. The intensities of these two bands are dependent on both the APTS concentration used in the preparation and the reaction time. The results are summarized as fol-lows. For the sample systems in which smaller APTS concentration were used, most of the NH2 groups of the aminopropyl segments are converted into the NH+ 3 groups on the surface, showing that the SiO-…H+NH2-type structure is predominantly stabilized on the surface of the silica gel. As the APTS concentration in the reaction mixture increases, the population of NH2 groups in the silane layer coated onto the surface increases. Interpretation of the CH stretch region further suggests that cyclic structures may be formed on the surface as a consequence of the formation of NH+ 3 groups.
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  • 7
    ISSN: 1435-1536
    Keywords: Key words Gemini surfactant ; Small-Angle Neutron-Scattering ; Micellar model
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract The microstructure of the micelles formed in aqueous solution by gemini surfactants with aromatic spacers, [Br(CH3)2N+(C m H2 m +1)-(Ph)-(C m H2 m +1)N+(CH3)2Br, m=8 and Ph = o-, m- or p-phenylenedimethylene] has been examined by small-angle neutron scattering. Aggregation of the gemini surfactants with an o-phenylenedimethylene spacer brings about formation of premicelles and small micelles at concentrations below the second critical micelle concentration, while above this concentration marked micellar growth and variation in shape occurs. It is suggested that the minimum aggregate formed at this critical micelle concentration may be the trimer or tetramer and that this result supports the mechanism of “gemini → submicelle → assembly” for micellar growth.
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  • 8
    ISSN: 1435-1536
    Keywords: Calf ; pregastric lipase ; tributyrin ; monoacid triglycerides ; Michaelis ; Menten parameters
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract The commercial extract from the oro-pharyngeal tissues of calf has been used as the source of pregastric lipase and has been processed to yield a partially purified sample of the pregastric lipase. The activity of this lipase against the short-chain lipid tributyrin has been determined over a range of pH and temperature values. Optimum pH conditions were within the range 5.7–6.4 and the optimum temperature was within 37–48 °C. The lipase was also used to catalyze the hydrolysis of monoacid triglycerides (C4∶0–C12∶0) at 40 °C, pH 6.0 and maximum activity was obtained against tributyrin (C4∶0). The values of the kinetic parameterK m increase with increasing carbon-chain length of the carboxylic moiety on the triglycerides, thus, indicating a preference for tributyrin under the stated conditions. The results are compared with results previously obtained utilising goat, kid and lamb pregastric lipases.
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  • 9
    ISSN: 1435-1536
    Keywords: Key words Long spacer ; bis (quaternaryammonium bromide) ; micelle ; Small-angle-neutron scattering
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract The microstructure of the normal micelles formed by dimeric surfactants with long spacers, [Br−(CH3)2N+(C m H2 m +1)-(CH2) S  -(C m H2 m +1)N+(CH3)2Br−, m = 10 and s = 8, 10 and 12], has been investigated by small-angle neutron scattering and compared with previously reported results for micelles of the same dimeric surfactants with shorter spacers (m = 10 and s = 2, 3, 4 and 6). It was found that for dimeric surfactants with long spacers (s = 8 and 10), both micellar growth and variation in shape occur to only a small extent, if at all, compared with dimeric surfactants with short spacers. However, for the dimeric surfactant with the longest spacer, s = 12, the extent of micellar growth and shape variation is also large. These results are due to the differences in conformation of dimeric surfactants with short spacers (s = 2–6) compared with that of the surfactants with long spacers (s = 8–12).
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  • 10
    ISSN: 1435-1536
    Keywords: Key words Raman spectra ; Sodium dialkylsulfosuccinates ; Hydrophobic chains ; Environment
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract  A homologous series of sodium dialkylsulfosuccinates (SDAS) has been synthesized with various chain lengths (dibutyl, dihexyl, diheptyl, dioctyl, dinonyl, didecyl, diundecyl and didodecyl). These compounds are straight-chain analogues for Aerosol-OT. Raman scattering spectra have been recordered for these SDAS compounds, both in the solid state and in aqueous solutions. These spectra are analyzed in detail in the CH stretch and CH2 deformation regions, and the results depend specifically on the length of the hydrocarbon chain. In particular, the longitudinal accordion-like vibrational modes coming from the all-trans n-alkyl chains have been investigated. For the SDAS dihydrates, all hydrocarbon chains take up an extended form, whereas for the monohydrates the tails tend to become disordered at the CH2-CH2 single bond close to the terminal methyl groups. It has also been confirmed that for the concentrated aqueous SDAS (sodium dibutylsulfosuccinate – sodium dioctylsulfosuccinate) samples preferential stabilization of the extended conformation of the hydrocarbon chain may occur.
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