Experimental Design Optimization of the Determination of Total Halogens in Coal by Combustion-Ion Chromatography

Determination of total halogens in coal was investigated with oxygen bomb combustion followed by ion chromatography. Experimental parameters were optimized by fractional factorial design and response surface methodology. Fractional factorial design was employed in screening experiments to evaluate t...

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Published inAnalytical letters Vol. 48; no. 16; pp. 2597 - 2612
Main Authors Sredović Ignjatović, Ivana D., Onjia, Antonije E., Ignjatović, Ljubiša M., Todorović, Žaklina N., Rajaković, Ljubinka V.
Format Journal Article
LanguageEnglish
Published Taylor & Francis 02.11.2015
Subjects
Chromatography
Coal
Combustion
Fractional factorial design
Halogens
Ion chromatography
Reduction (chemical)
Response surface methodology
Total coal halogens
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Abstract Determination of total halogens in coal was investigated with oxygen bomb combustion followed by ion chromatography. Experimental parameters were optimized by fractional factorial design and response surface methodology. Fractional factorial design was employed in screening experiments to evaluate the influence of the oxygen pressure, catalyst, absorption solution, reduction reagent, bomb cooling time, and a combustion aid on the combustion of coal in an oxygen bomb. Response surface methodology was conducted to further refine the results obtained by fractional factorial design and to define parameters for the procedure. The accuracy and precision of combustion with ion chromatography were evaluated by the use of two certified reference materials and by fortified in-house coal standards. The limits of detection and quantification for total halogens were 0.84 and 2.80 milligrams per kilogram, respectively, for 500 milligram samples. Ion chromatography provided relative standard deviations less than 4 percent, recoveries exceeding 95 percent, and was convenient. This method is recommended for routine determination of total halogens in coal because of its reliability.
AbstractList Determination of total halogens in coal was investigated with oxygen bomb combustion followed by ion chromatography. Experimental parameters were optimized by fractional factorial design and response surface methodology. Fractional factorial design was employed in screening experiments to evaluate the influence of the oxygen pressure, catalyst, absorption solution, reduction reagent, bomb cooling time, and a combustion aid on the combustion of coal in an oxygen bomb. Response surface methodology was conducted to further refine the results obtained by fractional factorial design and to define parameters for the procedure. The accuracy and precision of combustion with ion chromatography were evaluated by the use of two certified reference materials and by fortified in-house coal standards. The limits of detection and quantification for total halogens were 0.84 and 2.80 milligrams per kilogram, respectively, for 500 milligram samples. Ion chromatography provided relative standard deviations less than 4 percent, recoveries exceeding 95 percent, and was convenient. This method is recommended for routine determination of total halogens in coal because of its reliability.
Author Todorović, Žaklina N.
Onjia, Antonije E.
Rajaković, Ljubinka V.
Sredović Ignjatović, Ivana D.
Ignjatović, Ljubiša M.
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SubjectTerms Chromatography
Coal
Combustion
Fractional factorial design
Halogens
Ion chromatography
Reduction (chemical)
Response surface methodology
Total coal halogens
Title Experimental Design Optimization of the Determination of Total Halogens in Coal by Combustion-Ion Chromatography
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