Elsevier

Journal of Chromatography A

Volume 693, Issue 1, 17 February 1995, Pages 89-99
Journal of Chromatography A

Regular paper
Analysis of a mixture of linear and cyclic siloxanes by cryo-gas chromatography-Fourier transform infrared spectroscopy and gas chromatography-mass spectrometry

https://doi.org/10.1016/0021-9673(94)01115-UGet rights and content

Abstract

A mixture of linear and cyclic methylsiloxanes was analysed to characterize the different types of siloxane structures using gas chromatography (GC), mass spectrometry (MS) and Fourier transform infrared (FT-IR) spectroscopy. Siloxane structures are formed by hydrolysis of dimethyldichlorosilane under controlled conditions in technical applications. In the presence of methyltrichlorosilane or even trimethylchlorosilane, linear polydimethylsiloxanes and mono-, bi- or polycyclic methylsiloxanes are synthesized depending on the reaction conditions. The main structural units are (CH3)3SiO32, (CH3)2SiO and (CH3)SiO32. GC-MS may provide molecular mass information, but it is not able to identify isomeric structures, which are also formed in lower quantities by the mentioned reactions. Coupling GC with FT-IR enables the determination of group frequencies to assign specific structures. Thus, combination of GC with MS and FT-IR may be used in elucidating complex cyclosiloxane compounds. FT-IR measurements were performed with a Tracer unit.

References (14)

  • D.W. Scott

    J. Am. Chem. Soc.

    (1946)
  • W. Patnode et al.

    J. Am. Chem. Soc.

    (1946)
  • C.B. Hurd

    J. Am. Chem. Soc.

    (1946)
  • G. Garzó et al.

    Acta Chim. (Budapest)

    (1971)
  • G. Alexander et al.

    Chromatographia

    (1974)
  • J. Powell et al.

    Tech. Quart.

    (1991)
  • N.R. Smyrl et al.

    Appl. Spectros.

    (1992)
    N.R. Smyrl et al.

    Appl. Spectros.

    (1992)
There are more references available in the full text version of this article.

Cited by (20)

  • Siloxane adsorption on activated carbons: Role of the surface chemistry on sorption properties in humid atmosphere and regenerability issues

    2019, Chemical Engineering Journal
    Citation Excerpt :

    The appearance of this band shows that other siloxane species are desorbing from the samples. Table 7 gathers the characteristic IR bands of different linear and cyclic (gas phase) siloxanes in the 1300–800 cm−1 region [37–40]. From data in Table 7, the band at 1035 cm−1 can be unambiguously attributed to the asymmetric Si-O-Si stretch vibration of D3.

  • Physico-chemical properties of PDMS surfaces suitable as substrates for cell cultures

    2016, Applied Surface Science
    Citation Excerpt :

    Independently of the PDMS stiffness, the recorded infrared spectra do not show any significant differences in samples where the chemical bondings between benzophenone radicals and PDMS curing agent were formed. The observed bands were characterized for PDMS and were attributed as follows [65–67]. The band of wavenumbers of 2963 cm−1, 2904 cm−1 correspond to CH asymmetric deformation in SCH3 while the band of 1412 cm−1 is attributed to asymmetric bending in CH3 chemical groups [65].

  • Characterization of degradation products of poly[(3,3,3-trifluoropropyl)methylsiloxane] by nuclear magnetic resonance spectroscopy, mass spectrometry and gas chromatography

    2009, Polymer Degradation and Stability
    Citation Excerpt :

    Additionally, the negative ionization mode generally has the advantage of providing fewer background signals than the positive mode. GC coupled to a flame ionization detector (FID) or mass spectrometer was repeatedly employed for the quantification of cyclosiloxanes [38,41–44]. The FID is a perfect tool for this purpose, as it is very sensitive and quantitative for all members of a homologous series, as its response is proportional to the ring size.

View all citing articles on Scopus
View full text