Solid-phase extraction-gas chromatography-mass spectrometry using a fullerene sorbent for the determination of inorganic mercury(II), methylmercury(I) and ethylmercury(I) in surface waters at sub-ng/ml levels.
A novel, straightforward solid-phase extraction system for the determination of inorganic mercury and organomercury compounds in water is proposed. The analytes, in a buffer medium at pH 4.5, are sorbed as diethyldithiocarbamate complexes on a C60 fullerene column an subsequently eluted and derivatized with sodium tetra-n-propylborate in ethyl acetate. Following elution, 1 microl of extract is injected into a gas chromatograph-mass spectrometer system. The proposed gas chromatography-mass spectrometry speciation method exhibits a linear range of 4-1 ng/ml, and a detection limit of 1.5 ng/l (sample volume, 50 ml). Its repeatibility, as relative standard deviation (RSD) (from 11 standards containing 50 ng/l for each analyte), is ca. 7%. No interferences from metals ions, such as Zn2+, Fe3+, Sb3+, As3+, Pb2+, Ni2+, Cu2+, Sn2+, Co2+, Mn2+ and Cd2+ were encountered at concentrations 1000 times higher than those of the mercury compounds. The method was used for the speciation of inorganic mercury, methylmercury and ethylmercury in various types of water including sea and waste water.
Muñoz
J
J
Department of Analytical Chemistry, University of Córdoba, Annex C-3 Building, Campus of Rabanales, E-14071 Córdoba, Spain.
Gallego
M
M
Valcárcel
M
M
D005035:Ethylmercury Compounds / Q000032:analysis*; D037741:Fullerenes / Q000737:chemistry*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D008628:Mercury / Q000032:analysis*; D008767:Methylmercury Compounds / Q000032:analysis*; D012680:Sensitivity and Specificity; D014874:Water Pollutants, Chemical / Q000032:analysis*
D005035:Ethylmercury Compounds; D037741:Fullerenes; D008767:Methylmercury Compounds; D014874:Water Pollutants, Chemical; D008628:Mercury