title: Determination of monomethylmercury in low- and high-polluted sediments by microwave extraction and gas chromatography with atomic fluorescence detection.
abstract: The analysis of monomethylmercury (MMHg) in sediments is a difficult task because both very low concentrations and interconversion between species especially in highly polluted samples are frequent. This work features a general strategy for real sediment analysis with preconcentration and/or clean-up steps for both low- and high-polluted sediments to control these specific problems. The extraction conditions have been optimized using closed-vessel microwave-assisted heating with acidic extractants. The analysis has been carried out by the injection of ethylated derivatives of the analytes into a capillary gas chromatographic system coupled to fluorescence spectrometry. When using 6M HNO3, the most labile inorganic mercury fraction as well as MMHg were extracted from the sediment but there was still some inorganic mercury that remained un-extracted. MMHg was stable and quantitatively recovered by applying this procedure. The role of the labile inorganic fraction on artifact MMHg generation has been evaluated and it has been found to be highly variable depending on the sediments' geochemical characteristics. Therefore, for high-polluted sediments (inorganic mercury concentration above 500 ngg(-1)) a clean-up step with dichloromethane has been used before ethylation, whereas for low content samples, preconcentration under nitrogen stream at room temperature has been optimized. Both steps can be combined if necessary. MMHg content has been found in good agreement with the certified value for the reference materials (IAEA-405 and ERM-CC580).
authors.affiliation: Regional Institute for Applied Scientific Research, University of Castilla-La Mancha, E-13071 Ciudad Real, Spain.
authors.forename: J J
authors.initials: JJ
authors.lastname: Berzas Nevado
authors.forename: R C
authors.initials: RC
authors.lastname: Rodríguez Martín-Doimeadios
authors.forename: F J
authors.initials: FJ
authors.lastname: Guzmán Bernardo
authors.forename: M
authors.initials: M
authors.lastname: Jiménez Moreno
mesh_terms: D016477:Artifacts; D002138:Calibration; D002623:Chemistry Techniques, Analytical; D002849:Chromatography, Gas / Q000379:methods*; D004867:Equipment Design; D019015:Geologic Sediments; D008767:Methylmercury Compounds / Q000032:analysis*; D008872:Microwaves; D012015:Reference Standards; D015203:Reproducibility of Results; D012997:Solvents; D013050:Spectrometry, Fluorescence / Q000379:methods*; D013054:Spectrophotometry, Atomic / Q000379:methods*; D013696:Temperature
chemical_list: D008767:Methylmercury Compounds; D012997:Solvents