Gas Chromatography Columns Based on Functionalized Polymer for the Analysis of Catalytic Reaction Products |
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| Authors: | E Yu Yakovleva Y V Patrushev D P Ivanov I P Prosvirin |
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| Institution: | 1.Boreskov Institute of Catalysis,Novosibirsk,Russia;2.Novosibirsk State University,Novosibirsk,Russia |
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| Abstract: | For the first time in this work, two methods of modification of poly(1-trimethylsilyl-1-propyne) (PTMSP) and the possibilities of its application for the determination of catalytic reaction products are described. Aging of PTMSP is determined by three mechanisms: physical, chemical and mechanical effects. Free volume decreases, texture characteristics change, and partial oxidation of the polymer takes place in the structure of PTMSP. The chromatographic behavior of PTMSP, which was used for 18 months, differs significantly from the properties of the freshly prepared polymer. Thermal stability and chemical inertness are the main requirements for chromatographic materials. Therefore, two methods were used to stabilize the aging process. The first method consisted of preparing a mixed phase by adding disubstituted polyacetylene poly(1-phenyl-1-propyne) (PPP) to PTMSP. The resulting sorbent Chromosorb Р NAW?+?10 wt% (97% PTMSP?+?3% PPP) is efficient for solving a wide range of chromatographic tasks such as simultaneous analysis of hydrocarbons and sulfur-containing inorganic gases, analysis of chlorine-substituted methanes in CCl4 and thiophene in benzene, separation of hydrocarbons and aromatic compounds. It should be noted, the low selectivity of separation of oxygen-containing components on this sorbent. A second method of PTMSP modification, namely the oxidation treatment with nitrous oxide, is proposed. It was shown that the polymer is oxidized by means of its C=C double bond with the formation of ketone, carbonyl and hydroxyl groups. The increase in number of those groups in the polymer changed the polarity of PTMSP. The change in polarity of polymer led to the selectivity of separations, including oxygen-containing substances. Examples of separations of aliphatic and aromatic hydrocarbons, oxygen- and halogen-containing substances are presented. Chromatographic characteristics of the sorbent Chromosorb P NAW?+?10 wt% (97% PTMSP?+?3% PPP) and PTMSP oxidized by nitrous oxide are stable in the temperature range from 30 to 220 °C for at least 1.5 years of continuous operation. | |
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