The determination of boron in zirconium and zircaloy

In view of the use of these materials in nuclear technology, their boron concentration has a special significance. The concentration limit for nuclear applications amounts to approximately 0.1 fig/g, which means that here the determination of boron raises considerable problems. 

Emission spectrometry and spark source mass spectrometry are not considered for the same reasons as in 1.1.1. 

The development of photometric methods for the determination of boron in zirconium has to be seen in close relation to that of appropriate methods for the determination of boron in titanium. Therefore reference is also made to some methods developed for the analysis of boron in titanium, with the restriction however that only these studies will be considered which can be applied at the very low boron concentrations of interest here. 

For the determination of low boron amounts in titanium Codell and Norwitz (9) propose l.T-dianthrimide as reagent. The procedure is as follows  

MarJfenko (10) recommends brill ant-green for the analysis of boron in titanium and zirconium. For zirconium one proceeds as follows 0.1 g of finely divided material is dissolved by heating in 0.5 ml concentrated sulphuric acid and 0.25 g potassium sulphate in a special quartz vessel. 

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The method described was developed by Mortier et al. (38) for the determination of boron in doped zirconium (100, 20, 1 and 0.5 pig/g of boron), in undoped zirconium and in zircaloy. The conditions given can be used for all these materials. For the 100 and 20 f g/g samples, however, shorter irradiation and measuring times may be used and an instrumental determination is feasible if 6 MeV protons are used. Table IV-3 summarises the most important nuclear reactions of zirconium and its impurities or alloying elements with protons. For low boron concentrations Be must be separated chemically from the radionuclides produced. 

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