A Workflow for Uncertainty Assessment in Elemental Analysis of Archaeological Ceramics: A Case Study of Neolithic Coarse Pottery from Eastern Siberia

• Published in: Heritage Vol. 6; no. 5; pp. 4434 - 4450
• Main Authors: Pashkova, Galina V., Statkus, Mikhail A., Mukhamedova, Maria M., Finkelshtein, Alexander L., Abdrashitova, Irina V., Belozerova, Olga Yu, Chubarov, Victor M., Amosova, Alena A., Maltsev, Artem S., Demonterova, Elena I., Shergin, Dmitriy L.
• Format: Journal Article
• Language: English
• Published: Basel MDPI AG 01-05-2023
• Subjects: archaeological ceramics; Archaeology; Case studies; Ceramic materials; Ceramics; Clay; Comparative analysis; elemental analysis; Fluorescence spectroscopy; Grain size; Historic artifacts; Historic buildings & sites; ICP-MS; Mass spectrometry; Neolithic; Powders; Provenance; Raw materials; Sampling error; Scientific imaging; Sediments; SEM; WDXRF; X-ray spectroscopy; µXRF; Russia; Siberia
• ISSN: 2571-9408; 2571-9408
• DOI: 10.3390/heritage6050234

In this study, the assessment of uncertainties introduced at different stages of the elemental analysis of archaeological ceramics has been described using the example of the Neolithic pottery sherds from Popovsky Lug (eastern Siberia). To evaluate the uncertainty introduced by sampling due to ceramic heterogeneity, three original sherds were cut into small subsamples. Powdered subsamples (250–350 mg) were analyzed using wavelength-dispersive X-ray fluorescence and inductively coupled plasma mass spectrometry methods, and the variations between analytical results for independent subsamples were compared with the variations introduced during the analytical process (measurement and sample preparation). It was shown that 250–350 mg of ceramic is sufficient to obtain good reproducibility (2–15%) between separate subsamples for most major and trace elements, even for the heterogeneous Neolithic ceramics included in this study. The differing behavior of concentration variations in some elements was explained by measuring the ceramic cross-sections by scanning electron microscopy and micro-X-ray fluorescence spectrometry, as well as by the theoretic modeling of the sampling error. The described workflow can be useful in finding uncertainties in elemental analysis results, which may affect the interpretation of bulk chemical composition in ceramic provenance studies.