Headspace single drop microextraction of methylcyclopentadienyl-manganese tricarbonyl from water samples followed by gas chromatography-mass spectrometry |
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Authors: | Pereira Francisco Javier Pena Bendicho Carlos Kalogerakis Nicolas Psillakis Elefteria |
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Affiliation: | a Departamento de Química Analítica y Alimentaria, Facultad de Ciencias de Vigo, Universidad de Vigo As Lagoas-Marcosende, E-36200 Vigo, Spain b Department of Environmental Engineering, Technical University of Crete, Polytechneioupolis, GR-73100 Chania, Greece |
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Abstract: | Headspace single drop microextraction coupled to gas chromatography-mass spectrometry yielded a simple, fast and virtually solventless analytical 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 μl octane microdrop exposed for 20 min to the headspace of a 10 ml aqueous sample (15 ml vial) containing 20% (w/v) NaCl and stirred at 1250 rpm. The calculated calibration curves gave a high level of linearity for MMT with correlation coefficients >0.9995 after conducting a 3-day study. The limit of detection was calculated to be 0.21 μg l−1. The proposed method achieved an enrichment factor of the order of 2100 and a 53% recovery after extracting the spiked aqueous solution for 20 min under the optimized experimental conditions. The repeatability and intra-day reproducibility of the proposed method, expressed as relative standard deviation were 8.4 and 6.4%, respectively. Finally, analysis of spiked tap and wastewater samples revealed that matrix had little effect upon extraction. |
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Keywords: | Headspace SDME MMT GC-MS Liquid-phase microextraction |
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