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Determination of the Content of Sulfur of Coal by the Infrared Absorption Method with High Acccuracy

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The present paper reported the differential scanning calorimetry-thermogravimetry curves and the infrared (IR) absorption spectrometry under the temperature program analyzed by the combined simultaneous thermal analysis-IR spectrometer. The gas products of coal were identified by the IR spectrometry. This paper emphasized on the combustion at high temperature-IR absorption method, a convenient and accurate method, which measures the content of sulfur in coal indirectly through the determination of the content of sulfur dioxide in the mixed gas products by IR absorption. It was demonstrated, when the instrument was calibrated by varied pure compounds containing sulfur and certified reference materials (CRMs) for coal, that there was a large deviation in the measured sulfur contents. It indicates that the difference in chemical speciations of sulfur between CRMs and the analyte results in a systematic error. The time-IR absorption curve was utilized to analyze the composition of sulfur at low temperatures and high temperatures and then the sulfur content of coal sample was determined by using a CRM for coal with a close composition of sulfur. Therefore, the systematic error due to the difference in chemical speciations of sulfur between the CRM and analyte was eliminated. On the other hand, in this combustion at high temperature-IR absorption method, the mass of CRM and analyte were adjusted to assure the sulfur mass equal and then the CRM and the analyte were measured alternately. This single-point calibration method reduced the effect of the drift of the IR detector and improved the repeatability of results, compared with the conventional multi-point calibration method using the calibration curves of signal intensity vs sulfur mass. The sulfur content results and their standard deviations of an anthracite coal and a bituminous coal with a low sulfur content determined by this modified method were 0.345% (0.004%) and 0.372% (0.008%), respectively. The uncertainty (U, k=2) of sulfur contents of two coal samples was evaluated to be 0.019% and 0.021%, respectively. Two main modifications, namely the calibration using the coal CRM with a similar composition of low-temperature sulfur and high temperature sulfur, and the single-point calibration alternating CRM and analyte, endow the combustion at high temperature-IR absorption method with an accuracy obviously better than that of the ASTM method. Therefore, this modified method has a well potential in the analysis of sulfur content.
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Keywords: Accuracy; Chemical speciation; Coal; Drift; Sulfur; Uncertainty

Document Type: Research Article

Publication date: February 15, 2014

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  • Spectroscopy and Spectral Analysis, founded in 1981, is sponsored by the Chinese Central Iron & Steel Research Institute. "Spectroscopy and Spectral Analysis" has been indexed in SCI(1999), Ei(1992), MEDLINE(1999), and AJ (1999). "Spectroscopy and Spectral Analysis" publishes original contributions on various fields in Spectroscopy, including research results on laser spectroscopy, IR, Ramn, UV/Vis, Optical Emission, Absorption and Fluorescence spectroscopy, X-ray Fluorescence, and Spectrochemical Analysis, as well as Reseach paper, Research notes, Experimental Technique and Instrument, Review and Progress on the latest development of spectroscopy and spectrochemical anlysis, etc. "Spectroscopy and Spectral Analysis" is published monthly by Peking University Press with book sizes of large 16-mo format , and 292 pages per issue.
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