Abstract
Experimentally demonstrated advantages of stationary phase immobilization are considered, namely, prevention of thermal rearrangement, prevention of phase stripping, sharper peaks of solvent and major sample components, regeneration of columns by solvent washing, thick films produced from fluid phases, low bleeding rates, easy recoating and repeated coating to produce sandwich coatings. The cross-linking reaction which produces an immobilized stationary phase is strongly dependent on the structure of the stationary phase. OV-61 is representative of stationary phases having the maximum polarity allowing immobilization. The polarity limit will probably be shifted to higher values. Immobilization as a method of producing stable coatings on difficult to wet support surfaces is limited to support-stationary phase combinations providing nearly perfect wettability. The selection of a suitable peroxide for the cross-linking reaction is discussed. Based on arguments such as activity, cross-linking efficiency, influence of decomposition products, volatility, stability in solution, and safety of handling, a clear preference for a dialkyl peroxide, e.g., dicumyl peroxide, is indicated. Appropriate peroxide concentrations are discussed, and detailed instructions for the immobilization procedure are given. Particular attention is paid to solvent washing of the immobilized stationary phase columns.
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