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High-precision stable zirconium isotope ratio measurements by double spike thermal ionization mass spectrometry
Journal of Analytical Atomic Spectrometry ( IF 3.4 ) Pub Date : 2020-01-30 , DOI: 10.1039/c9ja00385a
Lanping Feng 1, 2, 3, 4, 5 , Wenfeng Hu 1, 2, 3, 4, 5 , Yu Jiao 1, 2, 3, 4, 5 , Lian Zhou 1, 2, 3, 4, 5 , Wen Zhang 1, 2, 3, 4, 5 , Zhaochu Hu 1, 2, 3, 4, 5 , Yongsheng Liu 1, 2, 3, 4, 5
Affiliation  

A new analytical method for the accurate and precise determination of stable zirconium isotope ratios in geological materials by thermal ionization mass spectrometry (TIMS) is presented. Isobaric interference from Mo was largely eliminated during filament heating and further reduced by off-line Mo interference correction. This methodology allows the complete elimination of Mo interference even with a Mo/Zr ratio up to 1. Separation of Zr from natural sample matrices was achieved by using a single DGA resin column with a small usage of acids (15 mL of 7 mol L−1 HNO3 and 3 mL of 1 mol L−1 HF). A 91Zr–96Zr double spike was admixed with samples before digestion, which enabled the correction of isotope fractionation that could occur during column separation and mass spectrometry measurement. The long-term measurement reproducibility of δ94Zr is generally better than ±0.06‰ (uncertainty represented by two standard deviations, hereinafter referred to as 2 SD), assessed by repeated analyses of Zr standard reference NIST SRM 3169 and eleven geological reference materials. The Zr isotope ratios of geological reference materials BHVO-2 and AGV-2 obtained in this study are consistent with the reported values measured by MC-ICP-MS, confirming the accuracy of the proposed method. This new method greatly simplifies the chemical separation process and is particularly suitable for Zr isotope analysis of complex matrix (especially for high Mo) samples.

中文翻译:

通过双峰热电离质谱法测量高精度稳定的锆同位素比率

提出了一种通过热电离质谱法(TIMS)准确,准确地测定地质材料中稳定的锆同位素比的新分析方法。Mo的等压线干扰在灯丝加热过程中已基本消除,并且通过离线Mo干扰校正进一步降低了。这种方法允许沫干扰完全消除即使是沫/ Zr的比高达1.从天然样品基质分离的Zr,通过使用单一的DGA树脂柱的酸的使用量小(15毫升7摩尔大号实现- 1 HNO 3和3 mL 1 mol L -1 HF)。一个91的Zr 96消化前将Zr双峰与样品混合,这可以校正在色谱柱分离和质谱测量过程中可能发生的同位素分馏。的长期测量的可重复性δ 94通过对Zr标准参考NIST SRM 3169和11种地质参考材料进行重复分析,得出Zr通常优于±0.06‰(不确定度由两个标准偏差表示,以下称为2 SD)。这项研究中获得的地质参考物质BHVO-2和AGV-2的Zr同位素比与MC-ICP-MS测得的报道值一致,证实了该方法的准确性。这种新方法大大简化了化学分离过程,尤​​其适用于复杂基质(尤其是高Mo)样品的Zr同位素分析。
更新日期:2020-01-30
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