An integrated approach based on oxidative pyrolysis and microwave-assisted digestion for the multi-elemental analysis of coal samples by ICP-based techniques
IR@NML: CSIR-National Metallurgical Laboratory, Jamshedpur
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Title |
An integrated approach based on oxidative pyrolysis and microwave-assisted digestion for the multi-elemental analysis of coal samples by ICP-based techniques
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Creator |
Krishna, M V B
Chandrasekaran, K Chakravarty, S Karunasagar, D |
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Subject |
Chemical Engineering
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Description |
Complete dissolution of the coal sample has been achieved using an integrated approach based on oxidative pyrolysis (OP) and microwave-assisted digestion (MWD) for the quantitative determination of major to ultra-trace elements by inductively coupled plasma (ICP)-based techniques. The coal samples were initially pyrolysed by heating to similar to 500 degrees C in the presence of an oxygen stream. Subsequently MWD was applied to the pyrolysed coal residue with an acid mixture of 8 mL of 20%HNO3 + 5%HF + 5%H2O2 or 20%HNO3 + 0.4%NH4HF2 + 5%H2O2. Analysis was carried out by ICP-MS (Be, V, Cr, Mn, Co, Ni, Cu, Zn, As, Rb, Sr, Mo, Cd, Sb, Cs, Ba, W, Tl, Pb, Th, U and REEs) and ICP-OES (Na, K, Ca, Mg, Fe, Al, Sc, Ti). Critical experimental parameters related to OP and MWD were optimized through the analysis of two standard reference materials (SRMs) NIST-1632d and NIST-2685b. Studies with NH4HF2 have demonstrated that it can be used as a replacement to the highly toxic HF for achieving quantitative recovery (> 95%) of most of the elements studied here. The optimized method was subsequently applied to Indian coal samples collected from different coal mines. (C) 2015 Elsevier Ltd. All rights reserved.
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Publisher |
Elsevier
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Date |
2015
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Type |
Article
PeerReviewed |
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Format |
application/pdf
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Identifier |
http://eprints.nmlindia.org/7271/1/skchakravarty-2015-Fuel.PDF
Krishna, M V B and Chandrasekaran, K and Chakravarty, S and Karunasagar, D (2015) An integrated approach based on oxidative pyrolysis and microwave-assisted digestion for the multi-elemental analysis of coal samples by ICP-based techniques. Fuel, 158 (IF-3.611). pp. 770-778. |
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Relation |
http://apps.webofknowledge.com/full_record.do?product=UA&search_mode=GeneralSearch&qid=2&SID=S1AnDO8z54Fzm5VlBuU&page=1&doc=1&cacheurlFromRightClick=no
http://eprints.nmlindia.org/7271/ |
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