Synthesis and analytical properties of a novel columnar metallomesogenic polymer.
A metallomesogenic side-chain polymer with copper carboxylato discotic units in stacks prepared by covalent bonding of 14-pentadecenoic acid, stearic acid and poly(methylhydrosiloxane) is described. The physico-chemical and thermal properties of both monomeric and polymeric metallomesogens were determined by elemental analysis, IR, polarizing optical microscopy, thermal gravimetric analysis and differential scanning calorimetry. The polymeric states showed a discotic lamellar phase at 50-95 degrees C and an ordered discotic hexagonal phase at 95-200 degrees C. By dynamic coating, the metallomesogenic polymer was crosslinked to the capillary wall via benzoyl peroxide. The wall-coated capillary columns (15 m x 0.25 mm I.D.) were used for the separation of phenols. Factors affecting the retention and the sample selectivity were examined. Van 't Hoff plots as a function of temperature indicated that phase transitions were occurring. Thermodynamic properties of the analytes in this system were also studied. For the determination of a mixture of 3-aminophenol, 2-chlorophenol, 2-nitrophenol, 4-nitrophenol, o-methylphenol, m-methylphenol, p-methylphenol, 2,4-dichlorophenol, 2,4-dimethylphenol, 2,4-dinitrophenol, 2,4,6-trichlorophenol, 2,4,6-trimethylphenol, 4-bromophenol, 3-methyl-4-chlorophenol, pentachlorophenol, and unsubstituted phenol, the calibration graphs for most phenols were linear over the range of 10-1000 microg 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 that could be detected.
Liu
C Y
CY
Department of Chemistry, National Taiwan University, Taipei.
Chen
J L
JL
Shiue
C C
CC
Liu
K T
KT
D002152:Calorimetry, Differential Scanning; D055598:Chemical Phenomena; D002627:Chemistry, Physical; D002849:Chromatography, Gas / Q000379:methods*; D003300:Copper / Q000737:chemistry*; D003432:Cross-Linking Reagents; D005227:Fatty Acids / Q000737:chemistry; D007202:Indicators and Reagents; D010636:Phenols / Q000032:analysis; D011108:Polymers / Q000138:chemical synthesis*; D012833:Siloxanes / Q000737:chemistry; D013229:Stearic Acids / Q000737:chemistry; D013816:Thermodynamics
C402372:14-pentadecenoic acid; D003432:Cross-Linking Reagents; D005227:Fatty Acids; D007202:Indicators and Reagents; D010636:Phenols; D011108:Polymers; D012833:Siloxanes; D013229:Stearic Acids; C402373:poly(methylhydrosiloxane); C031183:stearic acid; D003300:Copper