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随着毛细管色谱越来越广泛地应用于各种分析工作中,毛细管色谱柱的制备技术,成为一个值得重视和研究的问题。而制备毛细管柱是一个复杂且不易掌握的技术。近年来,我们研究了非极性交联毛细管色谱柱,已经取得了一些进展。比如容易制做,容易掌握,成活率比较高。在此基础上,我们又对甲基硅橡胶系列固定液中带有苯基的硅橡胶交联柱进行了研制,也获得了良好的效果。新选的固定液因含有苯基对引发剂形成的初级游离基有消耗作用,给交联制备带来很大的难度。但是苯基取代的硅氧烷在高温空气中的安定性比甲基硅氧烷好,这是由于苯核的共振稳定化,苯基不象脂肪族基团那样容易受到氧化。事实证明苯基交联柱的柱温可达360—370℃。
As capillary chromatography is more and more widely used in a variety of analytical work, the preparation of capillary columns has become a problem worthy of attention and research. The preparation of capillary column is a complex and difficult to master the technology. In recent years, we have studied non-polar cross-linked capillary columns and some progress has been made. Such as easy to make, easy to grasp, the survival rate is relatively high. On this basis, we also developed a silicone rubber cross-linked column with a phenyl group in the methyl silicone rubber fixing solution and also achieved good results. The newly selected fixative has a consumable effect due to the consumption of primary radicals formed by the phenyl group on the initiator, which poses a great difficulty for cross-linking preparation. However, the phenyl-substituted siloxane is more stable than methylsiloxane in high temperature air due to the resonance stabilization of the benzene nucleus, which is not easily oxidized like an aliphatic group. Phenyl cross-linked column proved the column temperature up to 360-370 ℃.