Methods development for the determination of methyl mercury in sediment samples using gas chromatography with atomic fluorescence detection

Abstract

An analytical method for methylmercury (MeHg) using gas chromatography with atomic fluorescence detection is studied. The instrumental system is made based on a old gas chromatograph interfaced with an atomic fluorescence detector which is specific to Hg, currently available in our lab. Operating parameters for the GC-AFS system are optimised and analytical performances of the system are verified by quality control chart for stability. MeHg in sediment is leached and extracted to dichloromethane (DCM) in the presence of nitric acid, potassium chloride and copper sulfate. DCM in the extract is purged and MeHg is back extracted to aqueous phase followed by ethylation with sodium tetraethylborate in acetate buffer pH 5.3 containing potassium oxalate. The ethylated MeHg is then extracted to hexane and injected to GC-AFS for quantitation. The instrumental detection limit and method detection limit are 0.5 pg MeHg and 0.029 ppb MeHg (as Hg), respectively. The method can be applied for the determination of MeHg in soil, sludge and sediment samples.