电感耦合等离子体质谱法测定核级海绵锆及锆合金中16种痕量杂质元素

Determination of 16 Trace Impurity Elements in Nuclear-Grade Sponge Zirconium and Zirconium Alloys by Inductively Coupled Plasma Mass Spectrometry

取样品0.600 0 g,加入10 mL水润湿后,用5 mL氢氟酸和5 mL硝酸溶解,用水定重至60.0 g。选择灵敏度高且干扰小的同位素,以标准加入法补偿基体效应制作工作曲线,在射频功率1 100 W,雾化气流量0.87 L·min^(-1)等条件下,采用电感耦合等离子体质谱法同时测定核级海绵锆及锆合金中16种杂质元素的含量。结果表明,16种元素的检出限(3s)为0.007~0.26μg·g^(-1)。测定核级海绵锆样品11次,各元素测定值的相对标准偏差(RSD)为2.2%~8.0%。按照标准加入法进行回收试验,回收率为90.0%~111%。

The sample(0.600 0 g) was wet in 10 mL of water, and dissolved in 5 mL of hydrofluoric acid and 5 mL of nitric acid. Water was added to the above solution to make the mass of solution attained to 60.0 g. The isotope with high sensitivity and small interference was selected, and the standard addition method was used to compensate the matrix effect in preparation of working curves. 16 impurity elements in nuclear-grade sponge zirconium and zirconium alloy were simultaneously determined by inductively coupled plasma mass spectrometry under the conditions of radio frequency power at 1 100 W and atomization gas flow rate at 0.87 L·min^(-1). As shown by the results, values of detection limit(3s) for 16 elements were in the range of 0.007-0.26 μg·g^(-1). The nuclear-grade zirconium sponge samples were determined 11 times, with RSDs of the determined values in the range of 2.2%-8.0%. Test for recovery was made by standard addition method, giving results in the range of 90.0%-111%.