Brinkkemper O, Braadbaart F, van Os B, van Hoesel A, van Brussel A A N, Fernandes R
Cultural Heritage Agency, PO Box 1600, 3800, BP, Amersfoort, The Netherlands.
Department of Earth Sciences-Geochemistry, Utrecht University, PO Box 80021, 3058, TA, Utrecht, The Netherlands.
Rapid Commun Mass Spectrom. 2018 Feb 15;32(3):251-261. doi: 10.1002/rcm.8033.
Isotopic analysis of archaeological charred plant remains offers useful archaeological information. However, adequate sample pre-treatment protocols may be necessary to provide a contamination-free isotopic signal while limiting sample loss and achieving a high throughput. Under these constraints, research was undertaken to compare the performance of different pre-treatment protocols.
Charred archaeological plant material was selected for isotopic analysis (δ C and δ N values) by isotope ratio mass spectrometry from a variety of plant species, time periods and soil conditions. Preservation conditions and the effectiveness of cleaning protocols were assessed through Fourier transform infrared spectroscopy and X-ray fluorescence (XRF) spectrometry. An acid-base-acid protocol, successfully employed in radiocarbon dating, was used to define a contamination-free isotopic reference. Acid-base-acid isotopic measurements were compared with those obtained from untreated material and an acid-only protocol.
The isotopic signals of untreated material and the acid-only protocol typically did not differ more than 1‰ from those of the acid-base-acid reference. There were no significant isotopic offsets between acid-base-acid and acid-only or untreated samples. Sample losses in the acid-base-acid protocol were on average 50 ± 17% (maximum = 98.4%). Elemental XRF measurements showed promising results in the detection of more contaminated samples albeit with a high rate of false positives.
For the large range of preservation conditions described in the study, untreated charred plant samples, water cleaned of sediments, provide reliable stable isotope ratios of carbon and nitrogen. The use of pre-treatments may be necessary under different preservation conditions or more conservative measurement uncertainties should be reported.
对考古烧焦植物残骸进行同位素分析可提供有用的考古信息。然而,可能需要适当的样品预处理方案,以提供无污染的同位素信号,同时限制样品损失并实现高通量。在这些限制条件下,开展了研究以比较不同预处理方案的性能。
从各种植物物种、时间段和土壤条件中选择烧焦的考古植物材料,通过同位素比率质谱法进行同位素分析(δC和δN值)。通过傅里叶变换红外光谱和X射线荧光(XRF)光谱法评估保存条件和清洁方案的有效性。一种在放射性碳测年中成功应用的酸碱酸方案被用于定义无污染的同位素参考。将酸碱酸同位素测量结果与未处理材料和仅用酸处理方案获得的结果进行比较。
未处理材料和仅用酸处理方案的同位素信号通常与酸碱酸参考信号的差异不超过1‰。酸碱酸与仅用酸处理或未处理样品之间没有显著的同位素偏移。酸碱酸方案中的样品损失平均为50±17%(最大值=98.4%)。元素XRF测量在检测污染更严重的样品方面显示出有希望的结果,尽管假阳性率很高。
对于本研究中描述的大范围保存条件,未处理的烧焦植物样品,经水清洗掉沉积物后,可提供可靠的碳和氮稳定同位素比率。在不同的保存条件下可能需要进行预处理,或者应报告更保守的测量不确定度。