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Supercritical fluid chromatography (SFC) of linear and cyclic components in technical silicone oils
(1994)
A simple SFE apparatus is presented. Particular emphasis is placed on the design of the restrictor, whereby the advantages of a special restrictor nozzle are discussed in relation to problems in conjunction with the use of capillary restrictors. The rubber additives, fullerenes and soil constituents used as example application underline the possibilities offered by the new restrictor presented here.
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.