HPLC separation of amines with a zirconia-based column coupled to a gas- phase chemiluminescence nitrogen specific detector (CLND)



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Texas A&M University


Gas phase chemiluminescence nitrogen specific detector (CLND)is used for the direct analysis of underivatized nitrogen-containing components such as alkylamines that can not be detected by the so called universal HPLC detector, the UV detector. However, alkali metal hydroxides can not be used as mobile phase constituents with the CLND because they form non volatile particulate combustion products that foul the detector. Therefore, trimethylsulfonium hydroxide (TMSOH) has been selected as a strong base for use with the CLND, because its combustion products, CO2, H2O and SxOy are volatile. An alkali-stable zirconia-based column was used and coupled to the CLND. Zirconia-based columns are mechanically and hydrolytically more stable than silica-based columns, which have a working pH range from 3 to 8 only. Zirconia-based columns can be used at a pH from 1 to 14 and can be used at temperatures up to 200?C. The separation of amines was carried out at high pH values where the amino groups were deprotonated. Primary, secondary, tertiary and quaternary amines were separated using a pH=13.7 mobile phase that contained only TMSOH, methanol and water. Good peak shapes were observed for all, except n-alkylamines and samples that contained both amino groups and alcohol groups.