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Beitrag zur Stickstoffbestimmung in keramischen Uranverbindungen

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Summary

The procedure for determining the nitrogen content in ceramic uranium compounds is reported. UN1+x (0≤x ≤0.80) and U(C,N) compounds with high N2 concentration as well as uranium carbides with nitrogen impurity content below 100 ppm were investigated. For determining the nitrogen content in the hightemperature nuclear fuels mentioned the conventional methods, such as the Kjeldahl and Dumas techniques and the vacuum-fusion method, have been modified and adapted to our problem.

The following results are discussed in detail:

  1. 1.

    The elimination of the main source of error with the Kjeldahl method: The low solubility of UN x compounds in conventional acid mixtures.

  2. 2.

    A modified Dumas method in which the CO2 carrier-gas takes part in a chemical reaction whereby nitrogen is quantitatively displaced. This method has been discovered by thermodynamical reasoning and its reliability has been proven by X-ray diffraction analysis. The addition of an oxidizing agent, such as CuO or KClO3, is unnecessary.

  3. 3.

    The determination of the composition of UN1+x compounds by hot extraction. The method is based on the parting of nitrogen from the UN1+x ; compound at temperatures above 1000° C in high vacuum with the formation of stoechiometrical UN.

The applicability of the three analytical methods is confirmed by the agreement of the nitrogen results within the error limits.

The coefficient of variation in the results yielded by the Dumas method, irrespective of the sample composition, is more favourable than that of the Kjeldahl method. The hot-extraction method also yields exact results when UN1+x compounds are analysed. By applying both the Dumas and the Kjeldahl method it is possible not only to determine quantitatively the nitrogen in nitride compounds but also the nitrogen in powdered materials, where it is possibly adsorbed in molecular form.

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Authors and Affiliations

  1. Institut für Reaktorwerkstoffe der Kernforschungsanlage Jülich, Deutschland

    A. Naoumidis, H. Nickel, J. Rottmann & H. J. Stöcker

Authors
  1. A. Naoumidis
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  2. H. Nickel
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  3. J. Rottmann
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  4. H. J. Stöcker
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Additional information

Vorgetragen auf dem Symposium über Reaktorchemie der GDCh in Jülich am 3. und 4.10.1966.

Die vorstehende Arbeit ist im Rahmen des THTR-Assoziationsvertrages zwischen der Europäischen Atomgemeinschaft, der Brown Boveri/Krupp Reaktorbau GmbH und der Kernforschungsanlage Jülich des Landes Nordrhein-Westfalen e.V. entstanden.

Für die tatkräftige Mithilfe bei den experimentellen Untersuchungen danken wir Frau J. Jansen und Herrn A. Schirbach.

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Naoumidis, A., Nickel, H., Rottmann, J. et al. Beitrag zur Stickstoffbestimmung in keramischen Uranverbindungen. Z. Anal. Chem. 226, 175–192 (1967). https://doi.org/10.1007/BF00502998

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  • DOI: https://doi.org/10.1007/BF00502998

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