Analytical Sciences

Abstract − Analytical Sciences, 26(9), 989 (2010).

Electrochemical Modification of a Graphite Platform for a Solid Sampling Electrothermal Atomic Absorption Spectrometry of Mercury
Department of Chemistry, Faculty of Science, Masaryk University, Kotlárská 2, Brno 611 37, Czech Republic
An electrodeposited palladium and iridium/gold mixture has been investigated as a chemical modifier for mercury determination in environmental samples by solid sampling electrothermal atomic absorption spectrometry. Electrochemical procedures of platform surface modification performed in a cell with 20 ml of solution, and in a drop of modifier solution have been optimized. Simple electrolysis in a drop was found to be the most consistent, taking the reproducibility as the major criterion. A total mass of 250 μg of electrodeposited palladium or an iridium/gold mixture was used. The lifetime of 60 – 70 firings for a deposited iridium/gold mixture was smaller than that for palladium with a lifetime of 100 – 120 firings. The detection limit was 120 pg Hg. Different sample masses of between 0.1 and 10 mg were weighed into modified platforms according to the mercury content. The results obtained for mercury in environmental samples as soils, sediments and plant, using solid sampling and calibration against aqueous standards stabilized by potassium permanganate, were in good agreement with those achieved by using the thermal deposition of modifiers and with measurements by pyrolysis atomic absorption spectrometry with gold amalgamation.