改性活性碳自组装多孔层毛细管气相色谱柱的研制及其特性评价

Preparation of the Phosphate Modified Charcoal Self-assembled PLOT Capillary Column for Gas-Solid Chromatography

摘要: 采用自组装膜制备技术和超细亚微米级吸附剂研制高效活性碳多孔层毛细管色谱柱(PLOT),选用K₃PO₄、K₂HPO₄和KH₂PO₄三种不同的磷酸盐对色谱柱进行改性脱活,考察了脱活盐浓度对色谱柱保留行为的影响程度,并采用研制的高效活性碳PLOT毛细管色谱柱对惰性气体和低碳烃(H₂、Air、CO、CO₂和C1～C4烃)进行了分离分析.结果表明:在高效活性碳PLOT毛细管色谱柱制备工艺中,活性碳吸附剂的最佳粒度为0.5～0.7μm之间;磷酸盐脱活剂的最佳浓度为1.5%,老化时间为250℃;所研制的高效活性碳PLOT毛细管色谱柱对惰性气体和低碳烃具有较好的分离度.

Abstract: A simple method for the preparation of submicron charcoal PLOT columns using fused silica capillaries by means of self assembled monolayerstechnology was reported. These columns were deactivated with K₃PO₄, K₂HPO₄ and KH₂PO₄ respectively, the retention behavior of the columns were evaluated, and used to separate inert gases and light hydrocarbons. The optimal range of pore size of charcoal particles used to prepare PLOT column was considered as 0.5～0.7 μm, the fitter conditional temperature and the favourable concetration of phosphate used to deactivate charcoal was 250℃ and 1.5% respectively.