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Detailed description of preparative synthetic method of ultra-pure odd n-alkanes is given. Both pentacosane and heptacosane were synthesized, respectively, from tridecanoic acid and tetradecanoic aci...d through ketene dimer. To obtain ultra-pure n-alkanes, the starting materials were purified as their esters through reverese liquid chromatography. Fractionation apparatus of the chromatography, suitable to preparative purpose, is described in some details. Gas chromatographic purities of the samples obtained were over 99.98%. Their phase transition behavior was examied by a heat-flux type DSC. Some effect of homologous impurities in the n-alkanes on the transition temperatures is reported.続きを見る
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