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Production of reference material

Determination of iron and silicon in certified reference iron ore samples by X-ray fluorescence (XRF) with high accuracy

Herstellung von Referenzmaterial

Bestimmung von Eisen und Silicium in zertifizierten Eisenerz-Referenzproben mit Hilfe von Röntgenfluorescenz hoher Richtigkeit

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Summary

Highly precise XRF was applied to certified reference iron ore samples. Interferences by matrix elements including strongly absorbing traces were eliminated by a preliminary multielement analysis and a subsequent addition of interfering elements to the synthetic reference samples. Results for Fe were compared with those of conventional potentiometric titration considering the interfering elements also in this case. Both methods were calibrated by a defined pure iron (99.970±0.003% Fe) and for XRF also by a very pure SiO2 (99.971±0.004% SiO2). A 1 to 1 correspondence of synthetic reference to analytical (replicated) samples was applied.

The results

  • exhibited a very close agreement between Fe values of XRF and titrimetry

  • confirmed previous findings by Boniface and Jenkins of a 0.14% (absolute) lower Fe level as compared to the certificates

  • were by 0.046% SiO2 ≃ 1% (relative) significantly higher than indicated in the certificates for the analyte Si.

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Authors and Affiliations

  1. A. G. der Dillinger Hüttenwerke, D-6638, Dillingen/Saar, Federal Republic of Germany

    Gotthard Staats

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  1. Gotthard Staats
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Staats, G. Production of reference material. Z. Anal. Chem. 327, 684–689 (1987). https://doi.org/10.1007/BF00489162

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  • DOI: https://doi.org/10.1007/BF00489162

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