Determination of methylmercury in sediments using supercritical fluid extraction and gas chromatography coupled with microwave-induced plasma atomic emission spectrometry

Determination of methylmercury in fish tissues by isotope dilution SPME-GC-ICP-MS

“…Determination of methylmercury in solid samples generally involves several analytical steps, including extraction, derivatization (where GC separation is involved), separation and detection. The most frequently used procedures for the extraction of mercury species from solid samples are based on alkaline [2][3][4][5][6] and acidic leaching, 7,8 aqueous distillation, [9][10][11][12][13] supercritical fluid extraction 14 and microwave-assisted extraction. [15][16][17] Grignard reagents, [18][19][20][21] sodium tetraethylborate (NaBEt 4 ), 17,[22][23][24][25][26] sodium tetrapropylborate (NaBPr 4 ) 18,27 and sodium tetraphenylborate (NaBPh 4 ) [28][29][30][31][32][33] have been used for efficient derivatization.…”

“…[15][16][17] Grignard reagents, [18][19][20][21] sodium tetraethylborate (NaBEt 4 ), 17,[22][23][24][25][26] sodium tetrapropylborate (NaBPr 4 ) 18,27 and sodium tetraphenylborate (NaBPh 4 ) [28][29][30][31][32][33] have been used for efficient derivatization. Gas chromatography, capillary electrophoresis or liquid chromatography are commonly used separation techniques for MMHg speciation in combination with atomic fluorescence spectrometry (AFS), 3,[34][35][36] electron-capture detection (GC-ECD), 37 atomic absorption spectrometry (AAS), 16,22 ion trap mass spectrometry, 30,31 inductively coupled plasma and microwave-induced plasma atomic emission spectrometry (ICP-AES, MIP-AES) 14,21,[38][39][40][41] and inductively coupled plasma mass spectrometry (ICP-MS) detection. 18,24,36,40,42,43 Over the past decade, the coupling of GC to ICP-MS has become a particularly popular technique for speciation work due to the high temporal resolution offered by GC and the high sensitivity, large dynamic range and multi-elemental capability of ICP-MS. On the other hand, sam...…”

Acoplamento cromatografia gasosa - espectrometria de absorção atômica em estudos de especiação: uma revisão

“…A maior parte dos sistemas visa o acoplamento direto da cromatografia, em linha, a técnicas de detecção diversas, como AAS, ICP-MS [10][11][12][13][14][15][16][17][18][19][20][21] , ICP-AES 10,22-29 , AFS30, MIP 10,21,[31][32][33][34][35][36][37][38][39][40][41][42][43][44][45][46] etc. Ou seja, os diferentes equipamentos relativos a essas técnicas analíticas tornam-se os detectores, postados à saída da coluna de separação.…”

Microwave-assisted extraction for methylmercury determination in sediments by high performance liquid chromatography-cold vapour-atomic fluorescence spectrometry

“…Methylmercury is separated by successive extractions with organic solvents (toluene or benzene) and back-extracted with an aqueous complexing agent (cysteine or thiosulfate). Other methodologies, such as alkaline digestion, 6-10 distillation 11,12 and supercritical fluid extraction 13 have been developed for the extraction of mercury species as alternatives to the Westö ö procedure. However, such sample preparation methods all suffer from some common disadvantages, such as laborious procedures, solvent-and timeconsuming problems and the possibility of originating artefacts.…”