An improved method for the preparation of immobilized stationary phases using radiation induced polymerization

Columns: Packed and Capillary; Column Selection in Gas Chromatography

“…Since then, various approaches for crosslinking have been investigated. These include chemical additives such as organic peroxides (120)(121)(122)(123)(124)(125)(126)(127)(128), azo compounds (82,129,130), ozone (131), and gamma radiation (77,(132)(133)(134)(135). Several different peroxides have been evaluated; dicumyl peroxide is the most popular.…”

“…On the other hand, for freeradical initiators that are liquid at ambient temperature, the column is first coated with stationary phase, then saturated with vapors of the reagent (47,82). Gamma radiation from a 60 Co source has also been used (77,114,(132)(133)(134)(135) as an effective technique for crosslinking polysiloxanes. In a comparative study of gamma radiation with peroxides, Schomburg et al (77) noted that each approach immobilized polysiloxanes, but that the formation of polar decomposition products is avoided with radiation.…”

Aspects of High-Resolution Gas Chromatography as Applied to the Analysis of Hydrocarbon Fuels and Other Complex Organic Mixtures. Volume 1

“…The coating procedures for glass tubes have been refined to a high degree and use both the static technique and the mercury plug dynamic process [337][338][339][340] . The recently developed immobilized stationary phases for glass OTCs have received considerable attention [341][342][343][344][345][346][347][348] and it appears that these types of phases will be used extensively in the future. Along with these advances, there have been several new procedures [349][350][351][352][353][354] for sealing the filled tube prior to removing the volatile solvent.…”

Azo compounds for free radical crosslinking of polysiloxane stationary phases

“…The by-products of their thermal decomposition have been shown to have undesirable effects on the activity and polarity of the crosslinked stationary phases [61. In this respect crosslinking with high energy radiation must be superior to thermal peroxidetreatment [12,13].lt hasalso beenshown that dicumyl peroxide causes oxidation during crosslinking of susceptible functional groups such as tolyl and cyanoAzo-ten-butane (ATB) has also been used as a free radical generator [6,141: ATB exhibits littleeffect on phase polarity and column activity while producing high levels of nonextractability. This paper reports the investigation of P~OPYI ~4 1 .…”