Analysis technology of high ionization potential element palladium by thermal ionization mass spectrometry

TANG Lei; LIU Xuemei; LONG Kaiming; YANG Tianli

doi:10.11889/j.0253-3219.2013.hjs.36.100203

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Analysis technology of high ionization potential element palladium by thermal ionization mass spectrometry

更新时间：2021-03-05

- Analysis technology of high ionization potential element palladium by thermal ionization mass spectrometry
- NUCLEAR TECHNIQUES Vol. 36, Issue 10, Article number: 100203(2013)
- 作者机构：
  
  中国工程物理研究院核物理与化学研究所
- 作者简介：
- 基金信息：
- DOI：10.11889/j.0253-3219.2013.hjs.36.100203
  CLC： O571.43
- Published：01 October 2013
- 稿件说明：
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[1]汤磊,刘雪梅,龙开明,杨天丽.高电离电位元素Pd的热表面电离质谱分析[J].核技术,2013,36(10):28-32.

TANG Lei, LIU Xuemei, LONG Kaiming, et al. Analysis technology of high ionization potential element palladium by thermal ionization mass spectrometry[J]. Nuclear techniques, 2013, 36(10): 100203
[1]汤磊,刘雪梅,龙开明,杨天丽.高电离电位元素Pd的热表面电离质谱分析[J].核技术,2013,36(10):28-32. DOI： 10.11889/j.0253-3219.2013.hjs.36.100203.

TANG Lei, LIU Xuemei, LONG Kaiming, et al. Analysis technology of high ionization potential element palladium by thermal ionization mass spectrometry[J]. Nuclear techniques, 2013, 36(10): 100203 DOI： 10.11889/j.0253-3219.2013.hjs.36.100203.

摘要

107Pd是长寿命裂变产物核素

有较大的分析价值。由于Pd的高电离电位（8.33 eV）

在热表面电离质谱（TIMS）的离子源内电离效率很低

因此

采用热表面电离质谱技术测量Pd的难度非常高。本文选择了三种激发剂对Pd的热电离质谱方法进行了改进

对比了TaF5、胶体石墨和磷酸硅胶等激发剂对Pd的质谱效率的影响。TaF5的效果要差于其他两种激发剂

胶体石墨和磷酸硅胶则效果相当

质谱效率在10–7量级。采用舟型带比单带的质谱效率提高了2倍以上

最高质谱效率达到4.55×10–7。测定了2 g Pd样品的同位素比值

采用磷酸硅胶为激发剂

106Pd/108Pd测量平均值与标称值偏差为0.36%

测量相对标准偏差为0.14%（n=10）

证明对于微克量级Pd样品的同位素比值测量可以获得较好的准确度与精度。

Abstract

Background:107Pd is an important long-lived fission product of Palladium isotope which is important in cosmology

nuclear technology and environmental studies. The analysis of Pd by Thermal Ionization Mass Spectrometry(TIMS) is difficult because Pd has high ionization potential(8.33 eV). Purpose: The paper attempts to improve mass efficiency of Palladium in TIMS. Methods: Three loading reagents including TaF5

colloidal graphite and phosphate silica-gel are compared. In the three loading reagents

colloidal graphite and phosphate silica-gel are better than TaF5

their mass efficiency can reach 10–7. Using V-type filament

the most of mass efficiency reaches4.55×10–7which is twice as high as that by using single filament. Results: The isotope ratio of 2- g Pd sample was measured with the loading reagent of phosphate silica-gel

106Pd/108Pd deviated 0.36% with standard value

RSD was0.14%(n=10). Conclusion: The experimental results show that the measurement of microgram Palladium sample can obtain good accuracy and precision by using appropriate loading reagents and V-type filament.

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