Simple methodology for methylmercury and inorganic mercury determinations by high-performance liquid chromatography–cold vapour atomic fluorescence spectrometry

• Published in: Analytica chimica acta 2001-12, Vol.448 (1), p.135-143
• Main Authors: Ramalhosa, E, Rı́o Segade, S, Pereira, E, Vale, C, Duarte, A
• Format: Article
• Language: English
• Subjects: Analysis methods; Analytical chemistry; Applied sciences; Chemistry; Chromatographic methods and physical methods associated with chromatography; Cold vapour atomic fluorescence spectrometry; Exact sciences and technology; Liquid chromatography; Methylmercury; Other chromatographic methods; Pollution; Simplex optimisation; Soil and sediments pollution; UV radiation
• ISSN: 0003-2670; 1873-4324
• DOI: 10.1016/S0003-2670(01)01317-4

An analytical methodology was developed to separate and quantify methylmercury (MeHg) and inorganic mercury by high-performance liquid chromatography (HPLC)–cold vapour atomic fluorescence spectrometry (CV-AFS). The use of UV oxidation of the organic forms of mercury, the tin(II) chloride reduction in acidic medium of mercury and the introduction of a water vapour trap based on H 2SO 4/CaCl 2 resulted in a low detection limit (DL) (10±2 pg, mean value±S.D.). The apparatus was operationally optimised through the modified simplex method leading to an increase of the signal by a factor of 2. The method performance has been tested by determining the MeHg concentration in a sediment certified reference material (CRM) and the results were statistically indistinguishable from the certificate value ( α=0.05) both for the mean value and S.D.