School of Archaeology, University of Oxford, Oxford, UK.
National Environmental Isotope Facility, British Geological Survey, Nottingham, UK.
Rapid Commun Mass Spectrom. 2022 Jul 30;36(14):e9318. doi: 10.1002/rcm.9318.
Embedding resins are commonly used to facilitate high-resolution sampling for stable isotope analysis but anomalous δ C values have been observed in some cases. Here we compare the results of microsampling strategies for hand-drilled versus resin-embedded micromilled samples from the same marine shells to assess whether resin contamination is implicated in δ C spikes. The comparison allows assessment of the relative benefits for spatial resolution, seasonal range for both δ O and δ C, and sample failure rates.
Hand-drilled samples were obtained from two bivalve shells (Spisula sachalinensis), corresponding to micromilled samples on the same shells where high δ C spikes were observed. All carbonate powders were analysed using a dual-inlet Isoprime mass spectrometer and Multiprep device. Results from both sample sets were compared statistically.
No anomalous high δ C values and no failures due to insufficient gas were observed in the hand-drilled samples in contrast to the embedded micromilled sequences. Spatial resolution was reduced (~2.5×) in the former compared with the latter, resulting in a small reduction in the total range observed in the micromilled δ C and δ O values. Reduced sampling resolution between the two datasets was only significant for δ O.
For S. sachalinensis (as with other similar bivalves), rapid growth mitigates the reduced sampling resolution of hand drilling and does not significantly impact observed isotopic range and seasonal patterning. Occurrence of anomalous δ C values were eliminated and failure rates due to insufficient sample size greatly reduced in the hand-drilled dataset. We can find no other explanation for the occurrence of δ C spikes than contamination by the embedding agent. We conclude that the logistical and interpretational benefits of careful hand drilling may be preferable to resin embedding for micromilling in marine shells, corals or speleothems where growth rate is rapid and the highest resolution is not required.
嵌入树脂常用于促进高分辨率采样以进行稳定同位素分析,但在某些情况下观察到异常的 δ C 值。在这里,我们比较了从相同的海洋贝壳中手动钻探与树脂嵌入微铣样品的微采样策略的结果,以评估树脂污染是否与 δ C 峰值有关。这种比较可以评估空间分辨率、δ O 和 δ C 的季节性范围以及样品失败率的相对优势。
从两个双壳贝类(Spisula sachalinensis)中获得手动钻孔样品,这些样品与在同一贝壳上观察到的高 δ C 峰值的微铣样品相对应。所有碳酸盐粉末均使用双入口 Isoprime 质谱仪和 Multiprep 设备进行分析。对两个样本集的结果进行了统计比较。
与嵌入的微铣序列相比,在手钻样品中没有观察到异常的高 δ C 值,也没有因气体不足而导致的失败。与后者相比,前者的空间分辨率降低了(约 2.5 倍),导致微铣 δ C 和 δ O 值观察到的总范围略有缩小。两个数据集之间的采样分辨率降低仅对 δ O 具有显著影响。
对于 S. sachalinensis(与其他类似的双壳类动物一样),快速生长减轻了手钻采样分辨率降低的影响,并且不会对观察到的同位素范围和季节性模式产生重大影响。在手钻数据集,异常的 δ C 值的出现被消除,并且由于样品尺寸不足而导致的失败率大大降低。除了嵌入剂的污染之外,我们找不到 δ C 峰值出现的其他解释。我们得出的结论是,在生长速度快且不需要最高分辨率的海洋贝壳、珊瑚或洞穴石笋中,精心手动钻探的逻辑和解释优势可能优于树脂嵌入微铣。