Boreskov Institute of Catalysis, Siberian Branch, Russian Academy of Sciences, Prospekt Lavrent'eva 5, 630090 Novosibirsk, Russia.
J Chromatogr A. 2013 Jul 12;1298:109-17. doi: 10.1016/j.chroma.2013.05.017. Epub 2013 May 21.
The chromatographic and adsorption properties of poly(1-trimethylsilyl-1-propyne) (PTMSP), a high permeable glassy polymer, were studied in the course of long-term usage of the Chromosorb P NAW+10wt% PTMSP adsorbent on a packed column in the temperature range of 30-180 °C. The structural changes in PTMSP related to a decrease in free volume and partial oxidation of the polymer were shown to substantially affect the adsorbent's properties. After the first 1.5 years (7000 h) of the column operation, the elution order of compounds changed, peak symmetry and efficiency of the column increased, the retention parameters as well as heats of adsorption of light hydrocarbons showed considerable changes. In order to stabilize the chromatographic properties of PTMSP, another disubstituted polyacetylene, poly(1-phenyl-1-propyne) (PPP), was added to the initial polymer, and a new mixed stationary phase, 97% PTMSP+3% PPP, was obtained and characterized. The resulting adsorbent, Chromosorb P NAW+10 wt% (97% PTMSP+3% PPP), is effective for solving a wide range of chromatographic problems, such as simultaneous detection of hydrocarbons and sulfur-containing inorganic gases, analysis of chlorine-substituted methanes in CCl4 and thiophene in benzene, separation of hydrocarbons and aromatic compounds. The chromatographic properties of the Chromosorb P NAW+10 wt% PTMSP (97% PTMSP+3% PPP) adsorbent were shown to remain stable in the course of its long-term operation (for at least 1.5 years, or 7000 h) on a packed column in the temperature range of 30-180 °C.
聚(1-三甲基硅基-1-丙炔)(PTMSP)是一种高渗透性的玻璃态聚合物,其色谱和吸附性能在 Chromosorb P NAW+10wt%PTMSP 填充柱上长期使用过程中(温度范围 30-180°C)进行了研究。研究表明,PTMSP 的结构变化与自由体积减少和聚合物部分氧化有关,这些变化会显著影响吸附剂的性能。在柱子运行的头 1.5 年(7000 小时),化合物的洗脱顺序发生了变化,峰形对称性和柱效提高,轻烃的保留参数和吸附热也发生了相当大的变化。为了稳定 PTMSP 的色谱性能,将另一种二取代的聚乙炔,聚(1-苯基-1-丙炔)(PPP)添加到初始聚合物中,得到并表征了一种新的混合固定相,97%PTMSP+3%PPP。所得吸附剂,Chromosorb P NAW+10wt%(97%PTMSP+3%PPP),可有效解决一系列色谱问题,如烃类和含硫无机气体的同时检测、CCl4 中氯取代甲烷和苯中噻吩的分析、烃类和芳烃的分离。Chromosorb P NAW+10wt%PTMSP(97%PTMSP+3%PPP)吸附剂在填充柱上(30-180°C 温度范围内)长期运行(至少 1.5 年或 7000 小时)过程中的色谱性能保持稳定。