Synthesis and analytical properties of a novel columnar metallomesogenic polymer

A metallomesogenic side-chain polymer with copper carboxylato discotic unit s in stacks prepared by covalent bonding of 14-pentadecenoic acid, stearic acid and poly(methylhydrosiloxane) is described. The physico-chemical and t hermal properties of both monomeric and polymeric metallomesogens were dete rmined by elemental analysis, LR, polarizing optical microscopy, thermal gr avimetric analysis and differential scanning calorimetry. The polymeric sta tes showed a discotic lamellar phase at 50-95 degrees C and an ordered disc otic hexagonal phase at 95-200 degrees C. By dynamic coating, the metallome sogenic polymer was crosslinked to the capillary wall via benzoyl peroxide. The wall-coated capillary columns (15 mx0.25 mm I.D.) were used for the se paration of phenols. Factors affecting the retention and the sample selecti vity were examined. Van 't Hoff plots as a function of temperature indicate d that phase transitions were occurring. Thermodynamic properties of the an alytes in this system were also studied. For the determination of a mixture of 3-aminophenol, 2-chlorophenol, 2-nitrophenol, 4-nitrophenol, o-methylph enol, m-methylphenol, p-methylphenol, 3-dichlorophenol 2,4-dimethylphenol, 2,4-dinitrophenol, 2,4,6-trichlorophenol, 2,4,6-trimethylphenol, 4-bromophe nol, 3-methyl-4-chlorophenol, pentachlorophenol, and unsubstituted phenol, the calibration graphs for most phenols were linear over the range of 10-10 00 mu g ml(-1) and the mass detection limits were in the ng range based on three times standard deviation of seven measurements of the lowest peak tha t could be detected. (C) 1999 Elsevier Science B.V. All rights reserved.