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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)3SiO1, (CH3)2SiO and (CH3)SiO3. 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.
Due to the utilisation of 1,1,2-trichlorotrifluoroethane (CFE) as extraction solvent the IR-spectrometric determination of total petrol hydrocarbon (TPH) in soil according to ISO/TR 11046 has been replaced by gas chromatography/flame ionisation detection (GC/FID) after extraction with a halogen-free solvent according to ISO/DIS 16703:2001. The results obtained with both methods by field laboratories in three proficiency testing (PT) rounds are compared. The consensus means obtained with GC/FID are typically 10%-20% (ranging between 0% and 25%) higher than those found with IR-spectroscopy. On the contrary, coefficients of variation (CV) are roughly double in case of GC/FID and are briefly discussed against the background of the Horwitz equation.