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Title: Determination of halogens in coal after digestion using the microwave-induced combustion technique

Abstract

The microwave-induced combustion (MIC) technique was applied for coal digestion and further determination of bromide, chloride, fluoride, and iodide by ion chromatography (IC). Samples (up to 500 mg) were combusted at 2 MPa of oxygen. Combustion was complete in less than 50 s, and analytes were absorbed in water or (NH{sub 4}){sub 2}CO{sub 3} solution. A reflux step was applied to improve analyte absorption. Accuracy was evaluated for Br, Cl, and F using certified reference coal and spiked samples for I. For Br, Cl, and F, the agreement was between 96 and 103% using 50 mmol L{sup -1} (NH{sub 4}){sub 2}CO{sub 3} as the absorbing solution and 5 min of reflux. With the use of the same conditions, the recoveries for I were better than 97%. Br, Cl, and I were also determined in MIC digests by inductively coupled plasma mass spectrometry, inductively coupled plasma optical emission spectrometry, and F was determined by an ion-selective electrode with agreement better than 95% to the values obtained using IC. Temperature during combustion was higher than 1350 {sup o}C, and the residual carbon content was lower than 1%. With the use of the MIC technique, up to eight samples could be processed simultaneously,more » and a single absorbing solution was suitable for all analytes and determination techniques (limit of detection by IC was better than 3 {mu} g g{sup -1} for all halogens).« less

Authors:
; ; ; ; ; ;  [1]
  1. Federal University of Santa Maria, Santa Maria (Brazil)
Publication Date:
OSTI Identifier:
21036906
Resource Type:
Journal Article
Journal Name:
Analytical Chemistry (Washington)
Additional Journal Information:
Journal Volume: 80; Journal Issue: 6; Journal ID: ISSN 0003-2700
Country of Publication:
United States
Language:
English
Subject:
01 COAL, LIGNITE, AND PEAT; COAL; HALOGENS; MICROWAVE HEATING; ION EXCHANGE CHROMATOGRAPHY; COMBUSTION; QUANTITATIVE CHEMICAL ANALYSIS; CHLORINE; BROMINE; FLUORINE; IODINE

Citation Formats

Flores, E M.M., Mesko, M F, Moraes, D P, Pereira, J S.F., Mello, P A, Barin, J S, and Knapp, G. Determination of halogens in coal after digestion using the microwave-induced combustion technique. United States: N. p., 2008. Web. doi:10.1021/ac8000836.
Flores, E M.M., Mesko, M F, Moraes, D P, Pereira, J S.F., Mello, P A, Barin, J S, & Knapp, G. Determination of halogens in coal after digestion using the microwave-induced combustion technique. United States. https://doi.org/10.1021/ac8000836
Flores, E M.M., Mesko, M F, Moraes, D P, Pereira, J S.F., Mello, P A, Barin, J S, and Knapp, G. 2008. "Determination of halogens in coal after digestion using the microwave-induced combustion technique". United States. https://doi.org/10.1021/ac8000836.
@article{osti_21036906,
title = {Determination of halogens in coal after digestion using the microwave-induced combustion technique},
author = {Flores, E M.M. and Mesko, M F and Moraes, D P and Pereira, J S.F. and Mello, P A and Barin, J S and Knapp, G},
abstractNote = {The microwave-induced combustion (MIC) technique was applied for coal digestion and further determination of bromide, chloride, fluoride, and iodide by ion chromatography (IC). Samples (up to 500 mg) were combusted at 2 MPa of oxygen. Combustion was complete in less than 50 s, and analytes were absorbed in water or (NH{sub 4}){sub 2}CO{sub 3} solution. A reflux step was applied to improve analyte absorption. Accuracy was evaluated for Br, Cl, and F using certified reference coal and spiked samples for I. For Br, Cl, and F, the agreement was between 96 and 103% using 50 mmol L{sup -1} (NH{sub 4}){sub 2}CO{sub 3} as the absorbing solution and 5 min of reflux. With the use of the same conditions, the recoveries for I were better than 97%. Br, Cl, and I were also determined in MIC digests by inductively coupled plasma mass spectrometry, inductively coupled plasma optical emission spectrometry, and F was determined by an ion-selective electrode with agreement better than 95% to the values obtained using IC. Temperature during combustion was higher than 1350 {sup o}C, and the residual carbon content was lower than 1%. With the use of the MIC technique, up to eight samples could be processed simultaneously, and a single absorbing solution was suitable for all analytes and determination techniques (limit of detection by IC was better than 3 {mu} g g{sup -1} for all halogens).},
doi = {10.1021/ac8000836},
url = {https://www.osti.gov/biblio/21036906}, journal = {Analytical Chemistry (Washington)},
issn = {0003-2700},
number = 6,
volume = 80,
place = {United States},
year = {Sat Mar 15 00:00:00 EDT 2008},
month = {Sat Mar 15 00:00:00 EDT 2008}
}