Abstract
Free radical cross-linking of methylpolysiloxane stationary phases to form insoluble rubbers recently became of widespread interest in capillary column gas chromatography. The use of various peroxides as free radical generators to form carbon—carbon cross-links in conventional stationary phases has been reported. In this study the applicability of various peroxids and azo compounds fro free radical cross-linking and the effects that these free radical generators have on commercially available stationary phases are described. Characteristics of the stationary phases such as chain length and functional groups and their roles in the cross-linking mechanism are discussed. The properties of benzoyl peroxide, dichlorobenzoyl peroxide, dicumyl peroxide, tert.-butylperoxide, and azo- tert.-butane as free radical generators were evaluated. Stationary-phase polarity change, column activity change and loss of stationary phase were all considered in the overall evaluation of the effectiveness of these free radical generators. Azo- tert.-butane showed minimal effect on phase polarity and column activity while benzoyl peroxide and dicumyl peroxide were the most effective in forming insoluble stationary phases.
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