Simple Mercury Fractionation In Biological Samples By Cv Aas Following Microwave-assisted Acid Digestion Or Tmah Pre-treatment

A simple and reliable method to determine total and inorganic mercury in biological certified reference material (CRM) by cold vapor atomic absorption spectrometry (CV AAS) is proposed. After the CRM treatment at room temperature with tetramethylammonium hydroxide (TMAH), inorganic mercury is determined by CV AAS. Total mercury is measured by the same technique, after sample acid digestion in a microwave oven. Organic mercury, basically methylmercury, is obtained by difference. In both procedures, the quartz tube is kept at room temperature. By means of analysis of the following reference materials: pig kidney, lobster hepatopancreas, dogfish liver and mussel tissue, it was clear that the difference between the total and inorganic mercury concentrations agrees with the methylmercury concentration. Only one calibration curve against aqueous standards in acidic medium was carried out for both procedures. The concentrations obtained by both procedures are in agreement with the certified values according to the t-test at a 95% confidence level. The relative standard deviations were lower than 3.0% for digested CRM and 6.0% for CRM treated with TMAH for most of the samples. The limits of detection in the samples were 0.02 μg g- 1 and 0.04 μg g- 1 for inorganic and total Hg, respectively, since the sample mass for total mercury was half of that for inorganic mercury determination. Simplicity and high efficiency without using chromatographic techniques are some of the qualities of the proposed method, being adequate for fractionation analysis of mercury in biological samples. © 2009 Elsevier B.V. All rights reserved.932206210Azevedo, F.A., (2003) Toxicologia do mercúrio, RiMa, São CarlosKaercher, L.E., Goldschmidt, F., Paniz, J.N.G., Flores, É.M.M., Dressler, V.L., Determination of inorganic and total mercury by cold vapor generation atomic absorption spectrometry using different temperatures of the measurement cell (2005) Spectrochim. Acta Part B, 60, pp. 705-710Vieira, M.A., Ribeiro, A.S., Curtius, A.J., Sturgeon, R.E., Determination of total and methylmercury in biological samples by photochemical vapor generation (2007) Anal. Bioanal. 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Spectrom., 14, pp. 1929-1931Willie, S.N., Grégoire, D.C., Sturgeon, R.E., Determination of inorganic and total mercury in biological tissues by electrothermal vaporization inductively coupled plasma mass spectrometry (1997) Analyst, 122, pp. 751-754Jimenez, M.S., Sturgeon, R.E., Speciation of methyl- and inorganic mercury in biological tissues using ethylation and gas chromatography with furnace atomization plasma emission spectrometric detection (1997) J. Anal. At. Spectrom., 12, pp. 597-601Torres, D.P., Vieira, M.A., Ribeiro, A.S., Curtius, A.J., Determination of inorganic and total mercury in biological samples treated with tetramethylammonium hydroxide by cold vapor atomic absorption spectrometry using different temperatures in the quartz cell (2005) J. Anal. At. 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Determination Of Mercury In Gasoline Diluted In Ethanol By Gf Aas After Cold Vapor Generation, Pre-concentration In Gold Column And Trapping On Graphite Tube

A simple method for the determination of mercury in gasoline samples diluted with ethanol by graphite furnace atomic absorption spectrometry (GF AAS) after cold vapor (CV) generation, pre-concentration in a gold column and trapping on a graphite tube is proposed. The methodology is based upon conventional analytical processes that can be performed by any laboratory with a chemical generation and gold amalgamation systems coupled to the atomic absorption spectrometer. The GF AAS temperature was optimized, being the retention, pyrolysis and atomization temperatures, respectively, 100°C, 150°C and 800°C. Gasoline samples were prepared simply by forming a 2-fold diluted solution in ethanol. The mercury formed vapors by reacting the sample with the reducing agent were pre-concentrated in a gold column and further retained on a graphite tube, coated with gold as permanent modifier. Five samples from different gas stations around the UFSC Campus (Florianópolis, Brazil) were analyzed and the Hg concentrations were found to be in the range from 0.40μgL-1 to 0.90μgL-1. Calibration against aqueous standard solutions in acidic medium was carried out. The standard solutions had about the same viscosity as the gasoline diluted in ethanol. The relative standard deviations were lower than 2.4% for the samples. The limits of detection in the samples were 0.08 and 0.14μgL-1, with and without pre-concentration in the gold column, respectively. The accuracy of the method was estimated by applying the recovery test and recovery values between 92 and 100% were obtained. A sample throughput of 4h-1 was achieved. Simplicity and high detection capability are some of the qualities of the method. © 2010 Elsevier B.V.9613236Saint'Pierre, T.D., Dias, L.F., Maia, S.M., Curtius, A.J., Determination of Cd, Cu, Fe, Pb and Tl in gasoline as emulsion by electrothermal vaporization inductively coupled plasma mass spectrometry with analyte addition and isotope dilution calibration techniques (2004) Spectrochim. Acta. Part B., 59, pp. 551-558Brandão, G.P., Campos, R.C., Luna, A.S., Determination of mercury in gasoline by cold vapor atomic absorption spectrometry with direct reduction in microemulsion media (2005) Spectrochim. Acta. Part B., 60, pp. 625-631Wilheim, S.M., Bloom, N., Mercury in petroleum (2000) Fuel Process. Technol., 63, pp. 1-27Saint'Pierre, T.D., Dias, L.F., Pozebon, D., Aucélio, R.Q., Curtius, A.J., Welz, B., Determination of Cu, Mn, Ni and Sn in gasoline by electrothermal vaporization inductively coupled plasma mass spectrometry, and emulsion sample introduction (2002) Spectrochim. Acta. 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Spectrom., 23, pp. 140-144Rivaro, P., Ianni, C., Soggia, F., Frache, R., Mercury speciation in environmental samples by cold vapour atomic absorption spectrometry with in situ preconcentration on a gold trap (2007) Microchim. Acta., 158, pp. 345-352Welz, B., Sperling, M., (1999) Atomic Absorption Spectrometry, , WILEY-VCH, Weinheim, GermanyConaway, C.H., Mason, R.P., Steding, D.J., Flegal, A.R., Estimate of mercury emission from gasoline and diesel fuel consumption, San Francisco Bay area, California (2005) Atmos. Environ., 39, pp. 101-105Won, J.H., Park, J.Y., Lee, T.G., Mercury emissions from automobiles using gasoline, diesel and LPT (2007) Atmos. Environ., 41, pp. 7547-7552Flores, E.M.M., Welz, B., Curtius, A.J., Determination of mercury in mineral coal using cold vapor generation directly from slurries, trapping in a graphite tube, and electrothermal atomization (2001) Spectrochim. Acta. Part B., 56, pp. 1605-161