摘要
测定锆及锆合金中杂质元素的研究较为常见,而针对高纯锆中化学成分检测的相关研究较少。在讨论各杂质元素质谱干扰的基础上,通过选择合适的同位素及分辨率,建立了辉光放电质谱法(GDMS)测定高纯锆中Na、Al、Si、P、Ti、V、Cr、Fe等36种痕量杂质元素的分析方法。对仪器参数进行了优化,最终选择氩气流量为370mL/min,放电电流为32mA,预溅射时间为15min。利用建立的实验方法对高纯锆样品中痕量杂质元素进行了测定,测定结果的相对标准偏差(RSD,n=7)均小于30%,质量分数大于0.1μg/g的杂质元素的RSD(n=7)均小于10%。采用电感耦合等离子体质谱法(ICP-MS)进行了方法比对,实验方法与ICP-MS的结果具有一致性。
The impurity elements in zirconium and zirconium alloy were commonly studied, but there were few reports on the analysis of chemical composition in high purity zirconium. On the basis of discussing the mass spectrometric interferences of various impurity elements, the determination method of 36 trace impurities such as Na, Al, Si, P, Ti, V, Cr and Fe in high purity zirconium by glow discharge mass spectrometry (GDMS) was established by selecting the proper isotopes and resolution rates. The instrumental parameters were optimized and the final conditions were selected: the argon flow rate was 370 mL/min, the discharge current was 32 mA, and the pre-sputtering time was 15 min. Trace impurity elements in high purity zirconium sample was determined according to the experimental method. The relative standard deviations (RSD, n =7) of determination results were less than 30%. For the impurity elements with mass fraction higher than 0.1 μg/g, the RSDs ( n =7) were all less than 10%. The determination results were compared with those obtained by inductively coupled plasma mass spectrometry (ICP-MS). The results showed good consistence.
作者
墨淑敏
王长华
李娜
潘元海
MO Shu-min;WANG Chang-hua;LI Na;PAN Yuan-hai(Guobiao (Beijing) Testing & Certification Co., Ltd., Beijing 100088, China)
出处
《冶金分析》
CAS
北大核心
2019年第5期13-18,共6页
Metallurgical Analysis
