Synthesis and characterization of 3,4-di(3-phenoxy-4-fluoro phenyl)-2,5-diphenyl phenyl grafted polysiloxane as stationary phase for gas chromatography
合成了一种耐高温的3,4-二(3-苯氧基-4-氟苯基)-2,5-二苯基苯基接枝聚硅氧烷(DPFP)固定相,使用静态涂渍法将其涂渍到毛细管柱内壁上,制成气相色谱柱。分离裂解乙烯的色谱图显示DPFP固定相在360℃时仍具有良好的分离能力。DPFP固定相的柱效为3 324块/米(保留因子(k)4.24,萘,0.25 mm i.d.)。麦克雷诺常数计算结果显示DPFP固定相属中等极性。溶剂化参数模型结果显示DPFP固定相与溶质之间的主要作用力为偶极-诱导偶极作用力、氢键碱性作用力。Grob试剂分离结果显示DPFP色谱柱具有良好的选择性与惰性。另外,芳香族同分异构体、苯取代物、多环芳烃、脂肪酸酯及脂肪醇都得到了良好的分离,表明DPFP固定相在应用方面有巨大的潜力。
【英文摘要】
A new high-temperature stationary phase called 3,4-di(3-phenoxy-4-fluoro phenyl)-2,5-diphenyl phenyl grafted polysiloxane(DPFP)was synthesized and statically coated on fused-silica capillary columns.The chromatogram of the polyethylene pyrolysis products showed that the DPFP column still owned good separation ability until 360 ℃. The column efficiency of the DPFP was 3 324 plates/m(retention factor(k)= 4. 24,naphthalene,0. 25 mm i. d.). McReynolds constants revealed that the polarity of the stationary phase...
【基金】
National Natural Science Foundation of China(No.21275090);
Technology Development Plan of Shandong Province(No.2014GGX107010)
【更新日期】
2017-06-19
【分类号】
O652.6
【正文快照】
In the past a few decades,capillary gas chro-matography(GC)has been widely used in petro-leum chemical industry,pesticide analysis andenvironment monitoring fields[1-4];differentkinds of polysiloxane stationary phases have beensynthesized to cater to the