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Chromatographic purification of antimony for accurate isotope analysis by MC-ICP-MS
Journal of Analytical Atomic Spectrometry ( IF 3.1 ) Pub Date : 2020-05-18 , DOI: 10.1039/d0ja00136h
Jianfeng Liu 1, 2, 3, 4, 5 , Jiubin Chen 5, 6, 7, 8 , Ting Zhang 5, 6, 7, 8 , Yina Wang 5, 7, 9, 10 , Wei Yuan 5, 6, 7, 8 , Yunchao Lang 5, 6, 7, 8 , Chenglong Tu 5, 11, 12, 13, 14 , Liangzhi Liu 5, 7, 10, 15 , Jean-Louis Birck 16, 17, 18, 19
Affiliation  

A two-step method for purifying antimony (Sb) from geological samples for accurate measurement of Sb isotopic composition using multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) was developed. Sb was separated from the matrix using two successive chromatographic columns loaded with AG 1-X4 and AG 50W-X8 resin, respectively. The separation method was calibrated using geological samples by assessing the extraction yield and the reproducibility of the measured isotopic composition, and resulted in a relatively low procedure blank and better recovery (98.7% ± 5.6%, n = 8, 2SD) compared to previous studies. The validation of the whole protocol, together with instrumental analysis, was confirmed by the investigation of the matrix effect and the result of a standard addition experiment. A combined sample-standard bracketing and external normalization (SSB-EN) method using cadmium (Cd) as an internal element was used for mass bias correction, which gave a reproducibility better than 0.04‰ (2SD). A variation of 0.29‰ of the δ123Sb value (relative to the NIST SRM 3102a standard) was observed in artificial and geological samples, implying the potential application of Sb isotopes in various environments.

中文翻译:

锑的色谱纯化,可通过MC-ICP-MS进行准确的同位素分析

建立了一种采用多收集器电感耦合等离子体质谱法(MC-ICP-MS)从地质样品中纯化锑(Sb)以便准确测量Sb同位素组成的两步​​法。使用分别装有AG 1-X4和AG 50W-X8树脂的两个连续色谱柱将Sb与基质分离。通过评估提取产率和所测同位素组成的重现性,使用地质样品对分离方法进行了校准,从而实现了相对较低的程序空白和更高的回收率(98.7%±5.6%,n= 8,2SD)。通过研究基质效应和标准加法实验的结果,证实了整个实验方案的有效性以及仪器分析结果。使用镉(Cd)作为内部元素的组合的样品标准包围和外部归一化(SSB-EN)方法用于质量偏差校正,其重现性优于0.04‰(2SD)。的0.29‰的变化δ 123在人工和地质样品中观察到的Sb值(相对于NIST SRM 3102A标准),这意味着Sb的潜在的应用在各种环境中的同位素。
更新日期:2020-07-08
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