Trace Determination of Hydrogen in Coke by Elemental Analysis

FH - HES

Authors

  • Romolo Cicciarelli
  • Basil Zuber
  • Christian Ambort

DOI:

https://doi.org/10.2533/000942902777680270

Keywords:

Coke and graphite, Elemental analysis, Gas chromatography, Recarburizer, Trace determination of hydrogen

Abstract

Recarburizers used in the steel industry are ruthlessly selected according to their quality. One of the critical parameters is the residual hydrocarbon content of the coke or graphite-based products. The current analytical procedure has a detection limit of about 0.2% hydrogen. The dynamic flash combustion of the sample coupled with gas chromatography (GC) was used to develop a simple method for the determination of hydrogen traces in coke. The sample was burned in an oxygen/helium atmosphere at 1020 °C. Separation of the combustion gases, NO2, CO2, H2O, and SO2, is accomplished on a chromatography column and measured by a thermal conductivity detector TCD. A linear response of hydrogen over a concentration range of 98–4910 mg kg?1 with a correlation coefficient of 0.9985 has been achieved. A detection limit of 26 mg kg?1 and a determination limit of 92 mg kg?1 were obtained with new equipment configurations and a sample weight of 8 mg. This corresponds to an impressive improvement of sensitivity of a factor of over 70. The coefficient of variation was found to be 31.3% at a concentration of 98 mg kg?1 and 0.7% at 4910 mg kg?1.

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Published

2002-06-01

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Section

Columns, Conference Reports

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