Quantitative analysis of 1‐olefins by programmed temperature gas chromatography

Gas chromatography has been extremely valuable for the analysis of materials used in the manufacture of surfactants. Temperature programming, which makes possible the efficient separation of wide boiling range mixtures, has extended the usefulness of the technique. In the work described, mixtures of 1‐olefins from C8蜢C18 in chain length were completely separated on a silicone rubber column in 17 min. The peaks were sharp, symmetrical and almost evenly spaced. A flame ionization detector was used. Using synthetic mixtures, it was found that over the C8蜢C18 range, peak area percent agrees very closely with weight percent. On a large number of measurements, the average deviation between area percent and weight percent was 0.5% absolute, with a range of ŷ2%. No bias in instrument response was observed with respect to chain length. Average carbon numbers calculated from chromatographic data were accurate to within ŷ0.2 units. Chromatographic results were compared with mass spectrometer data and were found to be significantly more precise and accurate. Furthermore, olefins could be detected in concentrations low enough that they were missed by the mass spectrometer (0.1%).