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Capillary supercritical fluid chromatography of aliphatic amines. Studies on the selectivity and symmetry with three different columns using carbon dioxide or nitrous oxide as mobile phase.

Journal of chromatography (1990-09-21)
O Gyllenhaal, J Vessman
ABSTRACT

The supercritical fluid chromatography of intact aliphatic amines with different columns is described. One group of amines was based on N,N-dimethyl-n-octylamine and related primary and secondary amines, and the other on the amino alcohol metoprolol and several of its analogues. Columns with three different phases were investigated, one non-polar coated with 5% phenyl methyl polysiloxane and two more polar with 25% cyanopropyl methylphenyl polysiloxane and Carbowax 20M. Generally, equal molar amounts were injected under splitless conditions and the peak symmetry was recorded. The system with the non-polar silicone phase was more inert, followed by the wax-phase column. The cyanopropyl column gave severe peak tailing although it was loaded with five times more of the amines than the other columns. The selectivity was investigated and was found higher with the two polar columns. Both showed a marked increase in the retention of amines with free hydrogens. With nitrous oxide the selectivity was almost the same as that with carbon dioxide as mobile phase. The nature of the flame ionization detector changed, however, giving a negative baseline drift on pressure programming. An interesting conclusion is that the amines are chromatographed as such with carbon dioxide as the mobile phase.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Silicone oil AR 20, viscosity ~20 mPa.s,   neat(25 °C)
Sigma-Aldrich
Silicone oil AP 100, viscosity ~100 mPa.s,   neat(25 °C)
Sigma-Aldrich
Poly(methylphenylsiloxane), viscosity 450-550 cSt 
Sigma-Aldrich
Silicone oil AR 200, viscosity ~200 mPa.s,   neat(25 °C)
Sigma-Aldrich
Silicone oil AP 1000, viscosity ~1000 mPa.s,   neat(25 °C)

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