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Headspace single drop microextraction of methylcyclopentadienyl-manganese tricarbonyl from water samples followed by gas chromatography-mass spectrometry

Elefteria Psillakis, Nicolas Kalogerakis, Francisco Javier Pena Pereira, Carlos Bendicho

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URI: http://purl.tuc.gr/dl/dias/85689CB1-F67B-4E88-BEAB-4DE82A71B668
Year 2007
Type of Item Peer-Reviewed Journal Publication
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Bibliographic Citation F. J.P. Pereira, C. Bendicho, N. Kalogerakis, E. Psillakis, "Headspace single drop microextraction of methylcyclopentadienyl-manganese tricarbonyl from water samples followed by gas chromatography–mass spectrometry",Talant.,vol, 74, no.1, pp. 47–51,2007.doi :10.1016/j.talanta.2007.05.024 https://doi.org/10.1016/j.talanta.2007.05.024
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Summary

Headspace single drop microextraction coupled to gas chromatography–mass spectrometry yielded a simple, fast and virtually solventlessanalytical protocol used for the headspace analysis of aqueous samples contaminated with methylcyclopentadienyl-manganese tricarbonyl (MMT).Initially, several experimental parameters were controlled and optimized and the optimum conditions found were 2.5 l octane microdrop exposedfor 20 min to the headspace of a 10ml aqueous sample (15 ml vial) containing 20% (w/v) NaCl and stirred at 1250 rpm. The calculated calibrationcurves gave a high level of linearity for MMT with correlation coefficients >0.9995 after conducting a 3-day study. The limit of detection wascalculated to be 0.21 g l−1. The proposed method achieved an enrichment factor of the order of 2100 and a 53% recovery after extracting thespiked aqueous solution for 20 min under the optimized experimental conditions. The repeatability and intra-day reproducibility of the proposedmethod, expressed as relative standard deviation were 8.4 and 6.4%, respectively. Finally, analysis of spiked tap and wastewater samples revealedthat matrix had little effect upon extraction.

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