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A trifluoropropyl‐containing silphenylene–siloxane terpolymer for high temperature gas chromatography
Author(s) -
Mayer Bernhard X.,
Rauter Walfried,
Kählig Hanspeter,
Zöllner Peter
Publication year - 2003
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200301575
Subject(s) - silanol , siloxane , chemistry , selectivity , polymer , capillary action , phase (matter) , gas chromatography , copolymer , chromatography , thermal stability , analytical chemistry (journal) , chemical engineering , materials science , organic chemistry , composite material , catalysis , engineering
Abstract A silanol terminated tetramethyl‐ p ‐silphenylene–3,3,3‐trifluoropropylmethyl, dimethyl siloxane terpolymer was prepared by a condensation reaction. Its chemical composition and microstructure were characterized by 1 H and 29 Si nuclear magnetic resonance spectroscopy. The polymer was coated on fused silica capillary columns in order to evaluate its gas chromatographic properties. At moderate temperatures its selectivity is similar to that of medium polarity stationary phases; at high temperatures, however, the interactions between stationary phase and unsaturated triacylglycerols are reduced to such an extent that the typical GC behavior of an apolar phase could be observed. Furthermore, the columns showed high separation efficiency and a good inertness of the fused silica surface. Relatively low column bleed permitted a maximum allowable operating temperature of 360°C. These capillary columns were used to determine the distribution of the carbon numbers of triacylglycerols in extracts of human subcutaneous adipose tissue. Thermal treatment of the columns at 400°C leads to a high degree of immobilization associated with reduced column bleed and a slightly changed selectivity, which indicates that a crosslinking process has taken place. Nevertheless, decreased separation efficiency and the thermal instability of the trifluoropropyl group would indicate that the capillary columns should be used at temperatures < 380°C.