Methylmercury extraction from aquatic sediments: A comparison between manual, supercritical fluid and microwave-assisted techniques

Abstract During recent decades the speciation of organomercurials has been a challenge to analytical laboratories dealing with environmental studies. Although easily detectable levels of organomercurials, and especially of methylmercury, are found in marine predators and biota, sediments are of fundamental interest as they provide a tool for assessing the impact of anthropogenic emissions on the environment. However, as in many other analytical problems, the sample-preparation stage has received less attention than the determination stage itself, although it is universally recognised that it determines the reliability of the analytical results. Recent developments in sample preparation have now been applied to the methylmercury problem. In this article a direct comparison is made between manual extraction, supercritical fluid extraction and microwave-assisted extraction. Each technique was used to extract methylmercury from polluted sediments. The efficiencies, merits and disadvantages of each technique are discussed.

[1]  R. Cela,et al.  Quality control in the routine analysis of methylmercury in biological and environmental materials using gas chromatography with electron capture detection , 1994 .

[2]  J E O'Reilly,et al.  Gas chromatographic determination of methyl and ethyl mercury: "passivation" of the chromatographic column. , 1982, Journal of chromatography.

[3]  B. Olson,et al.  In situ methylation of mercury in estuarine sediment , 1974, Nature.

[4]  A. Wasik,et al.  Purge-and-trap isothermal multicapillary gas chromatographic sample introduction accessory for speciation of mercury by microwave-induced plasma atomic emission spectrometry. , 1998, Analytical chemistry.

[5]  P. Sandra,et al.  Sodium tetra(n-propyl)borate: a novel aqueous in situ derivatization reagent for the simultaneous determination of organomercury, -lead and -tin compounds with capillary gas chromatography–inductively coupled plasma mass spectrometry , 1998 .

[6]  R. Cela,et al.  Optimization of methylmercury microwave-assisted extraction from aquatic sediments , 1997 .

[7]  M. Horvat,et al.  Working Methods Paper: Certification of methylmercury compounds concentration in marine sediment reference material, IAEA‐356 , 1994 .

[8]  H. Emteborg,et al.  Determination of methylmercury in sediments using supercritical fluid extraction and gas chromatography coupled with microwave-induced plasma atomic emission spectrometry , 1996 .

[9]  R. Cela,et al.  Study of the distribution of methylmercury and total mercury in grain size fractions of freeze-dried estuarine sediment samples , 1994 .

[10]  Jacqueline M.R. Bélanger,et al.  Microwave-assisted process (MAP™): a new tool for the analytical laboratory , 1994 .

[11]  H. Tao,et al.  Mercury speciation in natural gas condensate by gas chromatography-inductively coupled plasma mass spectrometry , 1998 .

[12]  Yuehe Lin,et al.  Supercritical fluid extraction and chromatography of metal chelates and organometallic compounds , 1995 .

[13]  R. Cela,et al.  Evaluation of capillary columns used in the routine determination of methylmercury in biological and environmental materials , 1992 .

[14]  R. Cela,et al.  Mercury speciation in raw sediments of the pontevedra estuary (Galicia‐Spain) , 1992 .

[15]  Nicolas S. Bloom,et al.  Comparison of distillation with other current isolation methods for the determination of methyl mercury compounds in low level environmental samples , 1993 .

[16]  K. Smit,et al.  Stability and reactions of mercury species in organic solution , 1998 .

[17]  R. D. Evans,et al.  Determination of artifactual formation of monomethylmercury (CH3Hg+) in environmental samples using stable Hg2+ isotopes with ICP-MS detection: Calculation of contents applying species specific isotope addition , 1997 .

[18]  P. Garrigues,et al.  Speciation analysis for organotin compounds in sediments by capillary gas chromatography with flame photometric detection after microwave-assisted acid leaching , 1995 .

[19]  J. A. Colman,et al.  Artifact formation of methyl mercury during aqueous distillation and alternative techniques for the extraction of methyl mercury from environmental samples , 1997 .

[20]  U. Harms Improvement of sample pretreatment for gas chromatographic determination of methylmercury in marine biota , 1994 .

[21]  O. Donard,et al.  Microwave-Assisted Leaching of Organotin Compounds from Sediments for Speciation Analysis , 1995 .

[22]  H. Emteborg,et al.  Speciation of mercury in human whole blood by capillary gas chromatography with a microwave-induced plasma emission detector system following complexometric extraction and butylation. , 1992, The Analyst.

[23]  P. Sandra,et al.  Sensitive, Simultaneous Determination of Organomercury, -lead, and -tin Compounds with Headspace Solid Phase Microextraction Capillary Gas Chromatography Combined with Inductively Coupled Plasma Mass Spectrometry , 1997 .

[24]  S. Rapsomanikis,et al.  Speciation of mercury and methylmercury compounds in aqueous samples by chromatography-atomic absorption spectrometry after ethylation with sodium tetraethylborate , 1991 .

[25]  A. Diego,et al.  Interferences during mercury speciation determination by volatilization, cryofocusing, gas chromatography and atomic absorption spectroscopy: comparative study between hydride generation and ethylation techniques , 1998 .

[26]  G. Westöö,et al.  Determination of methylmercury compounds in foodstuffs. I. Methylmercury compounds in fish, identification and determination. , 1966, Acta chemica Scandinavica.

[27]  P. Quevauviller,et al.  Improvements in methylmercury determination prior to the certification of two tuna fish materials , 1993 .

[28]  James H. Weber,et al.  Speciation of inorganic tin and alkyltin compounds by atomic absorption spectrometry using electrothermal quartz furnace after hydride generation , 1986 .

[29]  K. Ganzler,et al.  Microwave extraction. A novel sample preparation method for chromatography. , 1986, Journal of chromatography.