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Capillary Gas Chromatographic Separation of Carboxylic Acids Using an Acidic Water Stationary Phase

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Abstract

An acidic water stationary phase is used for the analysis of carboxylic acids in capillary gas chromatography (GC). Under regular pH 7 operating conditions, these analytes are largely ionized and elute poorly, if at all, from the water phase. However, by adjusting the phase to pH 2, it is found that various acids are neutralized and can be readily eluted and separated in the system. Sulfamic acid is found to provide a stable pH for the water phase over time, whereas hydrochloric acid and other more volatile additives quickly evaporate from the column. Under optimal low pH conditions, the acidic analytes yield good peak shape and are readily observed for masses investigated down to 5 ng on-column. By comparison, on a conventional non-polar capillary GC column, the same analytes display threefold more peak tailing and are not detected for masses below 30 ng on-column. Through altering the phase pH, it is found that the selectivity between certain analytes can be potentially enhanced depending on their respective pKa values and/or ionizability. The analysis of various different samples containing carboxylic acids is demonstrated and the results indicate that this approach can possibly offer unique and beneficial selectivity in such determinations.

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Acknowledgements

The authors are grateful to the Natural Sciences and Engineering Research Council of Canada (NSERC) for a Discovery Grant in support of this project.

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  1. Department of Chemistry, University of Calgary, 2500 University Drive, NW, Calgary, AB, T2N 1N4, Canada

    Ernest Darko & Kevin B. Thurbide

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  1. Ernest Darko
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  2. Kevin B. Thurbide
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Correspondence to Kevin B. Thurbide.

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This study was funded by an NSERC Discovery Grant.

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The authors declare no conflict of interest.

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This study does not involve any human or animal participants.

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Darko, E., Thurbide, K.B. Capillary Gas Chromatographic Separation of Carboxylic Acids Using an Acidic Water Stationary Phase. Chromatographia 80, 1225–1232 (2017). https://doi.org/10.1007/s10337-017-3333-z

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  • DOI: https://doi.org/10.1007/s10337-017-3333-z

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