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On-line post-column extraction in column liquid chromatography with electron-capture detection

Part I: Design and analytical characteristics

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Summary

A post-column extraction module has been used for the on-line coupling of conventional-size (4.6mm i.d.) reversed-phase liquid chromatography (PPLC) and electron-capture detection (ECD). Hexane and toluene were used as extraction solvents, while methanol turned out to be preferable to dioxane and acetonitrile as modifier in the aqueous eluent. In this system the ECD behaves as a concentration-sensitive detector. The band broadening in the evaporation interface, which connects the extraction module with the ECD, dominates the total post-column band broadening; it can be reduced to 3–4 sec by directing at least 0.25–0.30 ml/min (i.e. 25–30%) of the extraction solvent to the ECD. Optimal signal-to-noise ratios were observed if 30–60% of the extraction solvent is directed to the ECD. The noise levels are 5–10 times higher than in systems using a direct coupling of normal-phase LC or narrow-bore reversed-phase liquid chromatography to the ECD. Separations of phenylurea herbicides and chlorophenols demonstrate the applicability of the RPLC-extraction module-ECD system.

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Maris, F.A., Nijenhuis, M., Frei, R.W. et al. On-line post-column extraction in column liquid chromatography with electron-capture detection. Chromatographia 22, 235–240 (1986). https://doi.org/10.1007/BF02268765

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  • DOI: https://doi.org/10.1007/BF02268765

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