Analytical Chemistry p. 651 - 658 (1985)
Update date:2022-07-29
Topics:
Apfel, M. A.
Finkelmann, H.
Janini, G. M.
Laub, R. J.
Luehmann, B.-H.
et al.
The synthesis and characterization of a variety of mesomorphic (liquid-crystalline) side-chain polysiloxane (MEPSIL) solvents, said to be useful as gas chromatographic stationary phases, are described and discussed.The synthetic scheme is based upon the hydrosilation reaction that occurs when 4-(allyloxy)benzoyl esters are contacted with poly(methylsiloxane) in the presence of a dicyclopentadienylplatinum(II) catalyst, while product characterization is carried out by IR, NMR, GC, DSC, elemental analysis, and direct-observation hot-stage light-polarized microscopy.Selectivity of the MEPSIL phases is shown to differ very substantially from those exhibited by all other common GC solvents.The MEPSIL found overall to be the best suited as a GC stationary liquid exhibits a melting point of 139 deg C (k -> n) and a nematic/isotropic (n -> i) transition temperature of 319 deg C, while the practical operating limits of the material span 150 to in excess of 300 deg C.
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