Comparative study of hotplate wet digestion methods for the determination of mercury in biosolids

The re-use of biosolids is becoming increasingly popular for land applications. However, biosolids may contain elevated levels of metals and metalloids (including mercury) relative to background environmental concentrations. Consequently, reliable mercury analysis is important to allow classification of biosolids and to determine appropriate options for beneficial uses. This paper reports on a comparative study of 12 hotplate wet digestion methods for their suitability for the determination of mercury in biosolids. The methods were applied to mercury biosolids samples from four localities of two different sewage treatment plants in the State of Victoria, Australia. Samples were also spiked with methylmercury chloride and mercury sulphide to evaluate the Hg recovery in each hotplate digestion method. Aqua regia (HCl:HNO(3)=3:1), reverse aqua regia (HCl:HNO(3)=1:3), nitric, hydrochloric, sulphuric acid and their combinations with or without hydrogen peroxide were studied as wet digestion solutions. The method providing the best mercury recoveries was optimized. Under optimal conditions the corresponding analytical procedure consisted of 1h pre-digestion of 0.4 g biosolids sample with 10 ml reverse aqua regia with temperature increasing to 110 degrees C and 3h digestion at this temperature. In the last 10 min of the digestion step, 2 ml hydrogen peroxide were added to ensure complete decomposition of all mercury containing compounds. After filtering and dilution with deionised water (1:10), the concentration of mercury was determined by cold vapour atomic absorption spectrometry. It is expected, that the wet acid digestion method developed in this study will be also applicable to biosolids from other sewage treatment plants and to other types of solid mercury samples with elevated levels of organic matter.