Abstract
Boron carbide is widely used as industrial material, because of its extreme hardness, and as a neutron absorber. As part of a round-robin exercise leading to certification of a new reference material (ERM-ED102) which was demanded by the industry we analysed nitrogen in boron carbide by inert gas fusion analysis (GFA) and instrumental photon activation analysis (IPAA) using the 14N(γ,n)13N nuclear reaction. The latter approach is the only non-destructive method among all the methods applied. By using photons with energy below the threshold of the 12C(γ,n)11C reaction, we hindered activation of matrix and other impurities. A recently installed beam with a very low lateral activating flux gradient enabled us to homogeneously activate sample masses of approximately 1 g. Taking extra precautions, i.e. self-absorption correction and deconvolution of the complex decay curves, we calculated a nitrogen concentration of 2260 ± 100 μg g−1, which is in good agreement with our GFA value of 2303 ± 64 μg g−1. The values are the second and third highest of a rather atypical (non-S-shape) distribution of data of 14 round-robin participants. It is of utmost importance for the certification process that our IPAA value is the only one not produced by inert gas fusion analysis and, therefore, the only one which is not affected by a possible incomplete release of nitrogen from high-melting boron carbide.
Twin-Detector system for analyzing spatially extended samples
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Acknowledgments
This article is dedicated to Wolf Görner on the occasion of his 65th birthday. We thank Oskar Haase for providing the high-energy photon beam, Christian Rauch for assistance with the measurements, and Thomas Dudzus, Heinrich Kipphardt, and Peter Barth for discussing determinations of light elements. Three anonymous referees helped to substantially improve the quality of this paper.
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Merchel, S., Berger, A. Determination of nitrogen in boron carbide by instrumental photon activation analysis. Anal Bioanal Chem 388, 385–389 (2007). https://doi.org/10.1007/s00216-007-1217-z
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DOI: https://doi.org/10.1007/s00216-007-1217-z