A Capillary Column for the Gas Chromatographic Analysis of Dicyclopentadiene

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Abstract
The production of dicyclopentadiene (DCPD) is generally accompished by the dimerization of cyclopentadiene (CPD) which progresses rapidly at a temperature of approximately 100°C. The purity if the DCPD is dependent upon the quality of the CPD feedstock. There is no known commercial process for the synthesis of CPD; the available supply amounting to approximately 100 MM pounds per year is recovered from hydrocarbon cracking and coking processes. The dimerization is a Diels-Alder addition in which one CPD molecule acts as the conjugated diolefin and another as the dienophile. The ability of CPD to function in this dual capacity results in the production of numerous codimers when other olefins and conjugated diolefins are present with CPD in the feed to the dimerizer. Analytical methods for determining the purity of DCPD are complicated by the presence of these codimers. Several GLC analytical procedures using various liquid phases which include polyglycols and modified polyglycols have been reported for the analysis of CPD and DCPD. Dahmen reported an analytical procedure which included the analysis of some codimers of CPD with other C5 acyclic diolefins. The mass spectrometric analysis of DCPD is subject to the usual problems arising from the presence of isomers of different molecular types, as in this situation: bicyclics and hydroindenes. Acceptable analyses of DCPD samples containing impurities such as codimers of CPD and butadiene, isoprene, piperylenes, and methylcyclopentadienes have been accomplished using capillary columns having m-bis(m-phenoxyphenoxy) benzene with 2% Apiezon L (MBMA) as a liquid phase.

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