热稳定的气相色谱固定相的研究(Ⅱ)——二甲基、苯基、四苯基苯基硅氧烷混合聚合物固定相

A STUDY ON THE THERMOSTABLE STATIONARY PHASES FOR GAS CHROMATOGRAPHY(Ⅱ)——THE USE OF POLYMER PREPARED BY A MIXTURE OF DIMETHYLDICHLOROSILANE,PHENYLTRICHLOROSILANE AND TETRAPHENYLPHENYLTRIETHOXYSILANE AS STATIONARY PHASE

四苯基苯硅氧烷聚合物固定相具有较高的热稳定性,对正构烷烃有较好的色谱分离性能,但对正构醇类则不能分离。AT-Taiar等曾用C_(6)H_(5)SiCl_(3)、C_(18)H_(37)SiCl_(3)与CCl_(4)制备了混合硅氧烷聚合物,应用于气相色谱,获得较好的色谱分离性能。为改善四苯基苯硅氧炕聚合物固定相对醇类的色谱分离性能,制备了Me_(2)SiCl_(2)、C_(6)H_(5)SiCl_(3)、(C_(6)H_(5))4C_(6)HSi(OEt)_(3)的混合水解物和混合预聚合物(以下简称混合水解物和混合预聚物),并将它们制成固定相,研究了热稳定性和气相色谱行为。

The hydrolysate and prepoiymer of a mixture of dimethyldichorosilane,phenyltrichlorosilane and tetraphenylphenyltriethoxysilane were prepared.They were dissolved in benzene and then coated on the diatoma-ceous supports respectively.The coated support was heat-treated under a stream of nitrogen at 400℃ for 12 hours.The prepared column has been used at a temperature up to 270℃without bleeding and gave a number of HETP of 1200 plates per metre.A mixture of n-alkanes containing C_(7)-C_(30) could be well separated by the prepared column with the temperature programmed to 280℃.A mixture of n-alkanols containing C_(4)OH,C_(6)OH,C_(8)OH,C_(10)OH,C_(12)OH,C_(14)OH,C_(16)OH and C_(18)OH has been well separated also when the temperature was programmed to 250℃.n-C_(16)H_(3)4 and n-C_(10)OH have been quantitatively determined by the column.The effects of the surface properties of the supports,the weight percentage of the hydrolysate or prepoiymer used in preparing the column and the temperature of heat-treament are discussed.