离子交换-电感耦合等离子体质谱法测定锆锡合金中痕量杂质元素

doi:10.3964/j.issn.1000-0593(2020)08-2622-07

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Abstract Zircaloy has been widely applied in the nuclear industry for its excellent nuclear properties，in which the impurity element content is usually controlled at a very low level. Inductively coupled plasma mass spectrometry（ICP-MS）is an inorganic mass spectrometry for the simultaneous analysis of multiple elements and has widely been used in the metallurgical analysis. ICP-MS has such advantages as simple spectrogram and high sensitivity，but inevitably there is mass spectrum interference problems，which need to be solved by other auxiliary means. Matrix separation is required for all isotopes are interfered by polyatomic ions or isobars of Zr and Sn when Cd in zircaloy was determined by ICP-MS. A method for the determination of 11 trace impurity elements including Al，B，Mg in zircaloy by ICP-MS was developed，among which 6 elements such as Cd and Mg were separated and enriched by micro cation exchange column. The potential interference of ¹¹³In on ¹¹³Cd was corrected by the interference correction equation. Other impurity elements ions were directly determined by internal standard method without separation. Impurity ions such as Cd²⁺ in dilute hydrofluoric acid were adsorbed on the cation exchange column，while Zr forms a complex anion which was not adsorbed，thus impurity ions was separated from matrix elements and got enriched. The impurity ions were eluted with hydrochloric acid and detected by ICP-MS，thereby eliminating the interference of Zr on the determination of Cd. The experimental conditions for the separation of Cd and Zr were studied，including medium acidity，leaching acidity，elution acidity，sampling concentration and flow rate. The behavior of other impurity elements under the separation conditions obtained by an optimization experiment was also investigated. The results demonstrate that Mg，Mn，Co，Cu，Pb have similar behavior of separation and enrichment to Cd and can be determined simultaneously. The final separation conditions were as follows. 2 mL sample with concentration of 50 mg·mL^-1 was pumped with a flow rate of 2 mL·min^-1 （medium acidity was 0.5% hydrofluoric acid），then leached with 0.5% hydrofluoric acid for 9 min，and finally eluted with 10% hydrochloric acid for 4.5 min. The separation period of the method is about 15 min，and detection limit were 0.005 8~0.21 μg·g^-1. The recoveries ranged from 85% to 110%，and RSD is less than 5% for each element. The 11 impurity elements in Zr-zirlo zircaloy sample of nuclear grade were analyzed by this method，and the precision and accuracy of results both meet the requirements of corresponding product standard.

Key words：Cation exchange; Inductively coupled plasma mass spectroscopy; Zircaloy; Cadmium; Impurity elements

Received: 2019-07-12 Accepted: 2019-12-05

ZTFLH:

O657.63

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https://www.gpxygpfx.com/EN/10.3964/j.issn.1000-0593(2020)08-2622-07 OR https://www.gpxygpfx.com/EN/Y2020/V40/I08/2622

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