TY - JOUR A1 - Keidel, Frank A1 - Wachholz, Sigrid A1 - Just, Ulrich A1 - Geissler, H. A1 - Käppler, K. T1 - Analysis of a mixture of linear and cyclic siloxanes by cryo-gas chromatography-Fourier transform infrared spectroscopy and gas chromatography-mass spectrometry N2 - 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. PY - 1995 DO - https://doi.org/10.1016/0021-9673(94)01115-U SN - 0021-9673 VL - 693 IS - 1 SP - 89 EP - 99 PB - Elsevier CY - Amsterdam AN - OPUS4-1422 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Keidel, Frank A1 - Rühlmann, K. A1 - Jähnichen, S. A1 - Scheller, D. A1 - Scheim, U. ED - Andrianov, K. A. T1 - On the synthesis of siloxanes. XXIII. Synthesis and spectroscopic characterization of 2-functional 1,3-dioxa-2,4,7-trisilacycloheptanes N2 - A series of 2-functional 1,3-dioxa-2,4,7-trisilacycloheptanes was synthesized and characterized by means of 29Si NMR spectroscopy, gas chromatography, high performance liquid chromatography and gas chromatography-mass spectrometry. The signals were assigned to the various configurational isomers. This assignment was confirmed by independent synthesis of individual isomers. The sequence of the NMR signals of the all-cis and trans-trans isomers required for the determination of stereochemistry was found to be the same as that of the respective cyclotrisiloxanes. KW - Cylosiloxanes KW - Synthesis KW - Spectroscopic characterization PY - 1995 DO - https://doi.org/10.1016/0022-328X(95)05586-0 SN - 0022-328X SN - 1872-8561 VL - 505 IS - 1 SP - 29 EP - 36 PB - Elsevier CY - Amsterdam AN - OPUS4-1423 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Keidel, Frank A1 - Wachholz, Sigrid A1 - Just, Ulrich A1 - Geißler, Heinz A1 - Käppler, K. T1 - Analysis of siloxane pyrolysis products by cryo-GC/FT-IR and GC/MS PY - 1995 DO - https://doi.org/10.1007/BF00323377 SN - 0937-0633 VL - 352 IS - 5 SP - 515 EP - 520 PB - Springer CY - Berlin AN - OPUS4-1424 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Keidel, Frank A1 - Just, Ulrich A1 - Käppler, K. A1 - Scheim, U. T1 - Identification of low molecular vaporizable components in silicone resins using gas chromatography/mass spectrometry PY - 1996 SN - 0937-0633 IS - 354 SP - 21 EP - 26 PB - Springer CY - Berlin AN - OPUS4-1425 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Keidel, Frank A1 - Kretzschmar, Hans-Jürgen A1 - Weigel, Horst T1 - Isothiocyanatbildung bei der Schwefelvulkanisation mit Beschleunigern - Teil 2: Guanidinbeschleuniger PY - 1998 SN - 0948-3276 SN - 0022-9520 VL - 51 IS - 6 SP - 416 EP - 421 PB - Hüthig CY - Heidelberg AN - OPUS4-1426 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Keidel, Frank A1 - Just, Ulrich A1 - Wachholz, Sigrid A1 - Käppler, K. T1 - Characterization of linear, mono- and bicyclic methylsiloxanes by GC/MS and cryo-GC/FTIR T2 - InCom '95 CY - Düsseldorf, Germany DA - 1995-03-20 PY - 1995 AN - OPUS4-11107 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Keidel, Frank A1 - Just, Ulrich A1 - Wachholz, Sigrid T1 - Untersuchungen von Ozonreaktionen an Squalen als Modellsubstanz mittels MALDI/MS, GC/MS und GC/FTIR T2 - Analytica CY - Munich, Germany DA - 1996-04-23 PY - 1996 AN - OPUS4-11121 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Just, Ulrich A1 - Mellor, F. A1 - Keidel, Frank T1 - Supercritical fluid chromatography-mass spectrometry and matrix-assisted laser-desorption ionisation mass spectrometry of cyclic siloxanes in technical silicone oils and silicone rubbers N2 - Supercritical fluid chromatography in combination with mass spectrometry is used for determining cyclic siloxanes beside linear methyl and hydroxyl ''end-capped'' siloxanes. Electron impact ionisation and chemical ionisation techniques are utilized for identifying cyclic siloxanes in technical silicone oils and silicone rubber. Ammonia as reagent gas is preferred in the higher-molecular-mass range. Matrix-assisted laser-desorption ionisation mass spectrometry can be useful as a supplementary method for characterizing smaller amounts of both cyclic and linear siloxanes as well as silanols in the higher-molecular-mass range. PY - 1994 DO - https://doi.org/10.1016/0021-9673(94)00342-4 SN - 0021-9673 VL - 683 IS - 1 SP - 105 EP - 113 PB - Elsevier CY - Amsterdam AN - OPUS4-11260 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Keidel, Frank A1 - Just, Ulrich A1 - Wachholz, Sigrid A1 - Scheim, U. A1 - Käppler, K. T1 - Identifizierung von Siloxanpyrolysaten durch GC/MS und GC/FTIR T2 - InCom '94 CY - Düsseldorf, Germany DA - 1994-03-14 PY - 1994 AN - OPUS4-11172 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Just, Ulrich A1 - Mellor, F. A1 - Keidel, Frank T1 - Supercritical fluid chromatography (SFC) of linear and cyclic components in technical silicone oils PY - 1994 SN - 0937-0633 VL - 348 SP - 745 EP - 748 PB - Springer CY - Berlin AN - OPUS4-11350 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -