title: A 50% n-octylmethyl, 50% diphenyl-polysiloxane as stationary phase with unique selectivity for gas chromatography.
abstract: An n-octylmethyl, diphenyl-polysiloxane called SOP-50-Octyl was prepared by a condensation reaction of bis(dimethylamino) n-octylmethylsilane with diphenylsilanediol. The resulting copolymer was a gum with high molecular weight and was obtained with a yield of 80%. 1H and 29Si NMR spectroscopy revealed that the copolymer was a 52% octylmethyl, 48% diphenyl-polysiloxane with random microstructure. Small cyclic impurities could be almost quantitatively removed via a purification step. SOP-50-Octyl was used as stationary phase for the preparation of wall coated open tubular fused silica capillary columns for gas-liquid chromatography. The capillary columns exhibited high separation efficiency and high inertness. The stationary phase offered a unique selectivity due to its unique composition. The Rohrschneider-McReynolds constants indicated a low overall polarity in spite of the high phenyl content, as the polarity was distinctly decreased by the octyl substituent. Furthermore, the octyl substituent was responsible for a high column bleed, reducing the maximum allowable operating temperature to 280 degrees C. The elution temperatures of apolar compounds were increased due to increased interaction of the octyl substituent with the analytes. Some applications with volatile and semi-volatile organic compounds illustrate that SOP-50-Octyl is an excellent choice for confirmational analyses.
authors.affiliation: Department of Clinical Pharmacology, University School of Medicine, Vienna University, Währinger Gürtel 18-20, 1090 Vienna, Austria. Bernhard.Mayer@univie.ac.at
authors.forename: Bernhard X
authors.initials: BX
authors.lastname: Mayer
authors.forename: Hanspeter
authors.initials: H
authors.lastname: Kählig
authors.forename: Walfried
authors.initials: W
authors.lastname: Rauter
mesh_terms: D002849:Chromatography, Gas / Q000379:methods*; D009682:Magnetic Resonance Spectroscopy / Q000379:methods; D004364:Pharmaceutical Preparations / Q000737:chemistry; D011108:Polymers / Q000032:analysis / Q000138:chemical synthesis*
chemical_list: D004364:Pharmaceutical Preparations; D011108:Polymers