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Closed-vessel microwave digestion technique for lichens and leaves prior to determination of trace elements (Pb,Zn, Cu) and stable Pb isotope ratios
Authors:Alla Dolgopolova  Dominik J Weiss  Reimar Seltmann  Chris Stanley  Barry Coles  Andriy K Cheburkin
Institution:1. Department of Earth Science and Engineering , Imperial College London , Prince Consort Road, London, SW7 2BP, UK;2. Centre for Russian and Central Asian Mineral Studies (CERCAMS) , Department of Mineralogy, The Natural History Museum , Cromwell Road, London SW7 5BD, UK;3. Institute of Geological Sciences , 69-a Kabanbai Batyr St., 480100 Almaty, Kazakhstan a.dolgopolova@nhm.ac.uk;5. Centre for Russian and Central Asian Mineral Studies (CERCAMS) , Department of Mineralogy, The Natural History Museum , Cromwell Road, London SW7 5BD, UK;6. Centre for Russian and Central Asian Mineral Studies (CERCAMS) , Department of Mineralogy, The Natural History Museum , Cromwell Road, London SW7 5BD, UK;7. Institute of Environmental Geochemistry , University of Heidelberg , INF 236, D-69120 Heidelberg, Germany
Abstract:A reliable and robust procedure using closed-vessel microwave digestion of lichens and leaves for precise and accurate determination of trace elements (Pb, Zn and Cu) and stable Pb isotope ratios is presented. The method was developed using certified reference material CRM 482 Pseudovernia furfurea (Lichens), NIST 1515 (Apple Leaves) and NIST 1547 (Peach Leaves) and tested on lichens from a mining site in Russia. A mixture of 3?mL of HNO3, 3?mL of H2O2, 2?mL of H2O and 0.8?mL of HF ensured complete sample dissolution with 100?±?5% recovery for Pb, Zn and Cu at a maximum temperature of 210°C and pressure of 350?psi. The amount of HF and microwave pressure significantly influenced Pb, Zn and Cu recovery. Comparison between EMMA-XRF and ICP-AES showed a good correlation between Pb, Zn and Cu concentrations. Using the newly developed digestion method, Pb isotopes in lichens from the mining site were determined with an internal precision better than 0.02%.
Keywords:Microwave digestion  Acid decomposition  Standard reference materials (SRM)  Lichens  Solid particulates  Pb isotopes
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