Polar oligomeric polymer analysis by capillary super-critical fluid chromatography

Abstract

The analysis of the polar oligomers by capillary supercritical fluid chromatography coupled with a flame ionization detector (FID) is described. The mobile phase was CO2. Column temperature was increased stepwise from 60~170°C. A fused silica capillary column treated with polydimethy siloxane (3 m, 6. 5 m X 50 μm i.d.) was connected to a frit restrictor (25 cm X 50 μm i.d.). Samples were successfully chromatographed using pressure programming. Pressure was changed from 150 atm up to 400 atm at the FID temperature of 350°C. A surfactant such as polyethylene glycol alkylphenyl ether (Triton X-100) was analyzed at different column temperatures. It was found that the retention time of dichloromethane and sample peaks moved toward different directions as the temperature went up. The relative standard deviation (R.S.D.) for retention time of THF and Triton X-100 (14.3%) were within 0.5%. The R.S.D. for peak height of the highest peak of Triton X-100 was 6.3%. We obtained good results for polar oligomers such as m-cresol novolak resin by trimethylsilyl derivatization. The several peaks corresponding to the stereoisomers, as dimer, trimer, etc. inferred from FD-MS, were observed separately in SFC. © 1989, The Japan Society for Analytical Chemistry. All rights reserved.