High temperature stable OH‐terminated poly(3,3,3‐trifluoropropylmethylsiloxane/silphenylene) copolymer stationary phases for capillary gas chromatography

The unexpectedly good thermal stability of OH-terminated 3, 3, 3-trifluoropropylmethylsiloxane/silarylene copolymers can be attributed to both the inclusion of bulky aromatic units in the polysiloxane backbone and to an autocrosslinking process taking place at temperatures above 370°C, being specific for trifluoropropyl substituted polysiloxanes. The crosslinking mechanism is discussed. Both new OH-terminated phases, sildiphenylene/trifluoropropylmethyl and sildiphenylene ether/trifluoropropylmethyl-polysiloxane (SA-TF and SDPE-TF) were characterized, and their performance at high temperatures (>400°C) is demonstrated.

[1]  T. Welsch,et al.  The thermal immobilization of hydroxy-terminated silicone phases in high-temperature-silylated glass capillaries. A study of reaction mechanisms , 1991 .

[2]  R. Aichholz.  Preparation of glass capillary columns coated with OH-terminated (3,3,3-trifluoropropyl) methyl polysiloxane (PS 184.5) , 1990 .

[3]  G. Eglinton,et al.  Glass capillary gas chromatography-mass spectrometry at high temperatures. direct analysis of free base porphyrins and metal porphyrin complexes extracted from the serpiano oil shale , 1988 .

[4]  W. Blum.  Preparation of glass capillary columns coated with immobilized OV‐240‐OH (33% cyanopropyl substituted, OH‐terminated). An approach to improve the inertness and thermal stability of cyanoalkyl polysiloxane coatings , 1986 .

[5]  W. Blum.  Preparation of inert and high‐temperature stable apolar and medium polar glass‐capillary columns using OH‐terminated polysiloxane stationary phases , 1985 .

[6]  F. David,et al.  In situ gummification of methylphenylsilicones in fused-silica capillary columns , 1983 .

[7]  M. Lee,et al.  Static coating of capillary columns using mixed solvents , 1983 .

[8]  W. W. Wright,et al.  Thermal degradation of some fluorine-containing elastomers , 1982 .

[9]  L. Blomberg,et al.  Modification of glass capillary columns by cyclic (3,3,3‐trifluoropropyl)methylsiloxanes , 1980 .

[10]  K. Grob,et al.  Comprehensive, standardized quality test for glass capillary columns , 1978 .

[11]  N. Grassie,et al.  The thermal degradation of polysiloxanes—I. Poly(dimethylsiloxane) , 1978 .

[12]  T. Thomas,et al.  Thermal analysis of polydimethylsiloxanes. I. Thermal degradation in controlled atmospheres , 1969 .

[13]  E. Horning,et al.  A NEW LIQUID PHASE FOR GAS CHROMATOGRAPHIC SEPARATIONS OF STEROIDS , 1961 .