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Mercury determination and speciation analysis in surface waters

100%

Mladenova E., Dakova I., Tsalev D., Karadjova I.

Open Chemistry

2012

vol. 10

issue 4

1175-1182

A sorbent L-cysteine grafted silica gel has been evaluated for separation and enrichment of dissolved inorganic i-Hg(II) and methylmercury CH3Hg(I) from surface waters at sub-µg L−1 concentrations. Chemical parameters for mercury species enrichment and separation have been optimized. Analytical schemes for the determination of Hg species, using selective column solid phase extraction (SPE) with continuous flow chemical vapor generation atomic absorption spectrometry (CF-CVG-AAS) or inductively coupled plasma-mass spectrometry (ICP-MS) were developed. Possibilities for on-site SPE enrichment were demonstrated as well. The limits of quantification were 1.5 and 5 ng L−1 for dissolved i-Hg(II) and CH3Hg(I) by CF-CVG-AAS and 1 and 2.5 ng L−1 by ICP-MS with relative standard deviations between 7–12% and 7–14%, respectively. The chemically modified SPE sorbent has demonstrated high regeneration ability, chemical and mechanical stability, acceptable capacity and good enrichment factors. Results for total dissolved mercury were in reasonable agreement with those from independent analyses by direct ICP-MS determinations for river waters and for estuarine water certified reference material. [...]

Evaluation of various sample pre-treatment methods for total and inorganic mercury determination in biological certified reference materials by CVAAS technique

88%

Matusiewicz H., Stanisz E.

Open Chemistry

2010

vol. 8

issue 3

594-601

Sample preparation methods for non-separation cold vapor atomic absorption spectrometry (CVAAS) sequential inorganic mercury speciation in biological certified reference materials (CRMs) were investigated. The methylmercury concentration was calculated as the difference between total and inorganic mercury. Microwave-assisted decomposition method, and three ultrasonic extraction procedures based on acid leaching with HCl and HCOOH and solubilization with TMAH were employed as sample preparation methods. The replacement of a sample decomposition procedure by extraction prior to analysis by CVAAS, as well as the aspect of speciation analysis is discussed. The limits of detection in the sample were determined as 50 and 10 ng L−1 for inorganic and total mercury, which corresponds to absolute detection limits of 40 and 8 ng g−1 for inorganic and total mercury, respectively. The results were in good agreement with the 95% confidence level t-test of the certified values for total and inorganic mercury in the reference materials investigated. From the analysis of the CRMs, it was evident that the difference between the total and inorganic mercury concentrations agrees with the methylmercury concentration. The relative standard deviation was better than 11% for most of the samples. [...]

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2 Open Chemistry

1 2012

1 2010

1 Dakova I.

1 Karadjova I.

1 Matusiewicz H.

1 Mladenova E.

1 Stanisz E.

1 Tsalev D.

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Mercury determination and speciation analysis in surface waters

Evaluation of various sample pre-treatment methods for total and inorganic mercury determination in biological certified reference materials by CVAAS technique