聚苯撑基硅氧烷交联毛细管柱的研究

Study on Cross Linked Capillary Columns Coated with Polyphenylenesiloxane

使用静态涂渍法，在毛细管柱内壁涂渍新型苯撑基色谱固定液，通过原位交联，提高了液膜不可抽提性及稳定性。苯基通常被连接在聚硅氧烷硅原子的侧链上，如果两个硅原子之间通过苯联结而不是通过氧原子联结，则可形成聚苯撑基硅氧烷［１］，这种聚硅氧烷的弹性好。采用含５０％聚苯撑基硅氧烷研制出交联毛细管柱，并对制备过程重复程度进行了考察，评价了柱子的综合性能，简单介绍了柱子的极性及适用范围。

A new type of cross linked capillary column coated with polyphenylenesiloxane which possesses phenylene in the siloxane main chain has been described in this paper. The cross linking of polyphenylenesiloxane was performed in situ by the induction of DCUP. The structure of polyphenylenesiloxane is as followed:CH3SiCH3CH3OSiRRSiRROSiCH3CH3CH3nThe repeatabilities and solvent inextratabilities of the column preparations were investigated. For decane and 1 octanol, the values of n/L and k′ at 120℃ were 2800 3100 and 1.0 1.3, 2400 2800 and 5.0 6.0, respectively. The k′ values of the columns scarcely changed after eluting with methylene chloride and pentane. The base acid property was studied by analyzing 2,6 dimethylphenol and 2,6 dimethylaniline. Besides, in comparision with OV17 and OV25, the McReynolds′ constants of the cross linked column were also determined. The advantages of this kind of column are summarized as (1) easy preparation; (2) heat stability improved; and (3)good selectivity for the organic compounds which contain halogen, nitro group or phenol.