Determination of Se and Te in coal at ultra-trace levels by ICP-MS after microwave-induced combustion

Filipe S. Rondan, Alessandra S. Henn, Paola A. Mello, Magali Perez, Liam A. Bullock, John Parnell, Joerg Feldmann, Erico M. M. Flores, Marcia F. Mesko (Corresponding Author)

Research output: Contribution to journalArticle

Abstract

A method for ultra-trace determination of Se and Te in coal by inductively coupled plasma mass spectrometry (ICP-MS) was developed. Samples (up to 500 mg) were prepared by microwave-induced combustion (MIC) in a closed system pressurized with 20 bar of oxygen. Inorganic acids or their mixtures were evaluated as absorbing solution. Using HNO 3 + HCl (1 + 1), results obtained for Se and Te after sample preparation by MIC agreed with those obtained by reference methods, microwave-assisted wet digestion (MAWD) using concentrated HNO 3 and HF, and solid sampling electrothermal vaporization inductively coupled plasma mass spectrometry (SS-ETV-ICP-MS), and also with a certified reference material of coal (NIST 1632c) for Se. Very low limits of quantification (LOQ) were obtained: 0.002 and 0.007 mg kg -1 for Se and Te, respectively. Major elements were determined in final solutions obtained by MAWD and MIC, and their concentration in solutions of MIC was negligible (<10 μg L -1 ), minimizing the risk of interference in ICP-MS analysis. The proposed method was applied to samples of coal from the United Kingdom, with a wide range of inorganic composition (from 3 to 41% ash content), showing its robustness and feasibility for routine analysis. Se concentration ranged from 0.291 to 11.5 mg kg -1 , and Te was mainly found at ultra-trace levels (<0.007 to 0.11 mg kg -1 ). The proposed method presents several advantages over the reference methods, such as the use of a higher sample mass, low LOQs and, an important aspect, no need of using HF.

Original languageEnglish
Pages (from-to)998-1004
Number of pages7
JournalJournal of Analytical Atomic Spectrometry
Volume34
Issue number5
Early online date28 Feb 2019
DOIs
Publication statusPublished - 1 May 2019

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Inductively coupled plasma mass spectrometry
Coal
Microwaves
Ashes
Inorganic acids
Vaporization
Oxygen
Sampling
Chemical analysis

ASJC Scopus subject areas

  • Analytical Chemistry
  • Spectroscopy

Cite this

Determination of Se and Te in coal at ultra-trace levels by ICP-MS after microwave-induced combustion. / Rondan, Filipe S.; Henn, Alessandra S.; Mello, Paola A.; Perez, Magali; Bullock, Liam A.; Parnell, John; Feldmann, Joerg; Flores, Erico M. M.; Mesko, Marcia F. (Corresponding Author).

In: Journal of Analytical Atomic Spectrometry, Vol. 34, No. 5, 01.05.2019, p. 998-1004.

Research output: Contribution to journalArticle

Rondan, Filipe S. ; Henn, Alessandra S. ; Mello, Paola A. ; Perez, Magali ; Bullock, Liam A. ; Parnell, John ; Feldmann, Joerg ; Flores, Erico M. M. ; Mesko, Marcia F. / Determination of Se and Te in coal at ultra-trace levels by ICP-MS after microwave-induced combustion. In: Journal of Analytical Atomic Spectrometry. 2019 ; Vol. 34, No. 5. pp. 998-1004.
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title = "Determination of Se and Te in coal at ultra-trace levels by ICP-MS after microwave-induced combustion",
abstract = "A method for ultra-trace determination of Se and Te in coal by inductively coupled plasma mass spectrometry (ICP-MS) was developed. Samples (up to 500 mg) were prepared by microwave-induced combustion (MIC) in a closed system pressurized with 20 bar of oxygen. Inorganic acids or their mixtures were evaluated as absorbing solution. Using HNO 3 + HCl (1 + 1), results obtained for Se and Te after sample preparation by MIC agreed with those obtained by reference methods, microwave-assisted wet digestion (MAWD) using concentrated HNO 3 and HF, and solid sampling electrothermal vaporization inductively coupled plasma mass spectrometry (SS-ETV-ICP-MS), and also with a certified reference material of coal (NIST 1632c) for Se. Very low limits of quantification (LOQ) were obtained: 0.002 and 0.007 mg kg -1 for Se and Te, respectively. Major elements were determined in final solutions obtained by MAWD and MIC, and their concentration in solutions of MIC was negligible (<10 μg L -1 ), minimizing the risk of interference in ICP-MS analysis. The proposed method was applied to samples of coal from the United Kingdom, with a wide range of inorganic composition (from 3 to 41{\%} ash content), showing its robustness and feasibility for routine analysis. Se concentration ranged from 0.291 to 11.5 mg kg -1 , and Te was mainly found at ultra-trace levels (<0.007 to 0.11 mg kg -1 ). The proposed method presents several advantages over the reference methods, such as the use of a higher sample mass, low LOQs and, an important aspect, no need of using HF.",
author = "Rondan, {Filipe S.} and Henn, {Alessandra S.} and Mello, {Paola A.} and Magali Perez and Bullock, {Liam A.} and John Parnell and Joerg Feldmann and Flores, {Erico M. M.} and Mesko, {Marcia F.}",
note = "This study was financed in part by the Coordena{\cc}{\~a}o de Aperfei{\cc}oamento de Pessoal de N{\'i}vel Superior – Brasil (CAPES) – Finance Code 001. The authors are also grateful to the Conselho Nacional de Desenvolvimento Cient{\'i}fico e Tecnol{\'o}gico (CNPq, Grant 309297/2016-8), Instituto Nacional de Ci{\^e}ncia e Tecnologia de Bioanal{\'i}tica – INCTBio (CNPq Grant No. 573672/2008-3) and Funda{\cc}{\~a}o de Amparo {\`a} Pesquisa do Estado do Rio Grande do Sul (FAPERGS, Grant 16/2551-0000516-8) for supporting this study. Funding for the sample collection provided by the NERC Security of Supply programme UK (grant NE/L001764/1) is acknowledged.",
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T1 - Determination of Se and Te in coal at ultra-trace levels by ICP-MS after microwave-induced combustion

AU - Rondan, Filipe S.

AU - Henn, Alessandra S.

AU - Mello, Paola A.

AU - Perez, Magali

AU - Bullock, Liam A.

AU - Parnell, John

AU - Feldmann, Joerg

AU - Flores, Erico M. M.

AU - Mesko, Marcia F.

N1 - This study was financed in part by the Coordenação de Aperfeiçoamento de Pessoal de Nível Superior – Brasil (CAPES) – Finance Code 001. The authors are also grateful to the Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq, Grant 309297/2016-8), Instituto Nacional de Ciência e Tecnologia de Bioanalítica – INCTBio (CNPq Grant No. 573672/2008-3) and Fundação de Amparo à Pesquisa do Estado do Rio Grande do Sul (FAPERGS, Grant 16/2551-0000516-8) for supporting this study. Funding for the sample collection provided by the NERC Security of Supply programme UK (grant NE/L001764/1) is acknowledged.

PY - 2019/5/1

Y1 - 2019/5/1

N2 - A method for ultra-trace determination of Se and Te in coal by inductively coupled plasma mass spectrometry (ICP-MS) was developed. Samples (up to 500 mg) were prepared by microwave-induced combustion (MIC) in a closed system pressurized with 20 bar of oxygen. Inorganic acids or their mixtures were evaluated as absorbing solution. Using HNO 3 + HCl (1 + 1), results obtained for Se and Te after sample preparation by MIC agreed with those obtained by reference methods, microwave-assisted wet digestion (MAWD) using concentrated HNO 3 and HF, and solid sampling electrothermal vaporization inductively coupled plasma mass spectrometry (SS-ETV-ICP-MS), and also with a certified reference material of coal (NIST 1632c) for Se. Very low limits of quantification (LOQ) were obtained: 0.002 and 0.007 mg kg -1 for Se and Te, respectively. Major elements were determined in final solutions obtained by MAWD and MIC, and their concentration in solutions of MIC was negligible (<10 μg L -1 ), minimizing the risk of interference in ICP-MS analysis. The proposed method was applied to samples of coal from the United Kingdom, with a wide range of inorganic composition (from 3 to 41% ash content), showing its robustness and feasibility for routine analysis. Se concentration ranged from 0.291 to 11.5 mg kg -1 , and Te was mainly found at ultra-trace levels (<0.007 to 0.11 mg kg -1 ). The proposed method presents several advantages over the reference methods, such as the use of a higher sample mass, low LOQs and, an important aspect, no need of using HF.

AB - A method for ultra-trace determination of Se and Te in coal by inductively coupled plasma mass spectrometry (ICP-MS) was developed. Samples (up to 500 mg) were prepared by microwave-induced combustion (MIC) in a closed system pressurized with 20 bar of oxygen. Inorganic acids or their mixtures were evaluated as absorbing solution. Using HNO 3 + HCl (1 + 1), results obtained for Se and Te after sample preparation by MIC agreed with those obtained by reference methods, microwave-assisted wet digestion (MAWD) using concentrated HNO 3 and HF, and solid sampling electrothermal vaporization inductively coupled plasma mass spectrometry (SS-ETV-ICP-MS), and also with a certified reference material of coal (NIST 1632c) for Se. Very low limits of quantification (LOQ) were obtained: 0.002 and 0.007 mg kg -1 for Se and Te, respectively. Major elements were determined in final solutions obtained by MAWD and MIC, and their concentration in solutions of MIC was negligible (<10 μg L -1 ), minimizing the risk of interference in ICP-MS analysis. The proposed method was applied to samples of coal from the United Kingdom, with a wide range of inorganic composition (from 3 to 41% ash content), showing its robustness and feasibility for routine analysis. Se concentration ranged from 0.291 to 11.5 mg kg -1 , and Te was mainly found at ultra-trace levels (<0.007 to 0.11 mg kg -1 ). The proposed method presents several advantages over the reference methods, such as the use of a higher sample mass, low LOQs and, an important aspect, no need of using HF.

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