Sulfur isotope analyses using 3× elemental analysis/isotope ratio mass spectrometry: Saving helium and energy while reducing analytical time and costs

IF 1.8 3区 化学 Q4 BIOCHEMICAL RESEARCH METHODS
Jorge E. Spangenberg, Alice Bosco-Santos
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引用次数: 0

Abstract

Rationale

Helium (He) and energy shortages have caused price increases and reduced their availability. Using three combustion reactions per acquisition of carbon and nitrogen isotope ratios saves 50% He and energy during the elemental analysis/isotope ratio mass spectrometry (EA/IRMS). This approach needs to be tested for sulfur isotope (δ34S) analyses.

Methods

A new method to measure δ34S in three sequential combustion reactions within one EA/IRMS acquisition was developed. The same material or blank samples could be used in the three reactions. After SO2 was used, a N2 purging method was employed to prolong the lifetime of the valves in the EA/IRMS interface. The 3×EA/IRMS was applied to measure δ34S in precious samples, such as Ag2S from acid-volatile and chromium-reducible sulfur extracted with a multiple-port setup.

Results

The 3×EA/IRMS-δ34S method was validated with replicate analyses of international reference materials and laboratory standards with a wide range of mineralogical compositions and δ34S values. The method provided a strategic advantage for the δ34S measurements of small precious samples (measured between blanks). The accuracy and precision of the 3×EA/IRMS values effectively matched those obtained using conventional EA/IRMS, with good agreement between the mean ± SD values and the recommended values with their uncertainties.

Conclusions

Compared with the conventional EA/IRMS, the proposed method provides accurate and precise δ34S measurements of the sulfate and sulfide samples while saving approximately 50% of He, energy, SO2 reference gas, O2, analysis time, and cost. Notably, 3×EA/IRMS can provide up to three δ34S values unaffected by memory effects.

Abstract Image

利用 3× 元素分析/同位素比质谱法进行硫同位素分析:节省氦气和能源,同时减少分析时间和成本。
理由:氦气(He)和能源短缺导致价格上涨,减少了氦气的供应。在进行元素分析/同位素比质谱分析(EA/IRMS)时,每次采集碳和氮同位素比使用三次燃烧反应可节省 50%的氦气和能源。这种方法需要在硫同位素(δ34S)分析中进行测试:方法:开发了一种在一次 EA/IRMS 采集中测量三个连续燃烧反应中 δ34S 的新方法。三个反应可使用相同的材料或空白样品。使用 SO2 后,采用 N2 吹扫法延长 EA/IRMS 接口阀门的使用寿命。3×EA/IRMS 被用于测量贵重样品中的δ34S,如用多端口装置从酸挥发性和铬还原性硫中提取的 Ag2S:结果:3×EA/IRMS-δ34S 方法通过对具有多种矿物成分和δ34S 值的国际参考材料和实验室标准物质的重复分析进行了验证。该方法为小型贵重样品的 δ34S 测量(在空白之间测量)提供了战略优势。3×EA/IRMS 值的准确度和精确度与使用传统 EA/IRMS 所获得的值有效匹配,平均值 ± SD 值与推荐值及其不确定度之间具有良好的一致性:结论:与传统的 EA/IRMS 相比,所提出的方法能准确测量硫酸盐和硫化物样品的 δ34S 值,同时节省约 50% 的 He、能源、SO2 基准气体、O2、分析时间和成本。值得注意的是,3×EA/IRMS 可提供多达三个不受记忆效应影响的 δ34S 值。
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来源期刊
CiteScore
4.10
自引率
5.00%
发文量
219
审稿时长
2.6 months
期刊介绍: Rapid Communications in Mass Spectrometry is a journal whose aim is the rapid publication of original research results and ideas on all aspects of the science of gas-phase ions; it covers all the associated scientific disciplines. There is no formal limit on paper length ("rapid" is not synonymous with "brief"), but papers should be of a length that is commensurate with the importance and complexity of the results being reported. Contributions may be theoretical or practical in nature; they may deal with methods, techniques and applications, or with the interpretation of results; they may cover any area in science that depends directly on measurements made upon gaseous ions or that is associated with such measurements.
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