Instrumentation ancient periods

Trace elemental analysis of ancient ceramics has been proven a very useful tool for tracing the circulation of this material. Instrumental neutron activation analysis (INAA) was for years the analytical technique of choice to measure the composition of ceramics because of the large number of elements it could determine and its good sensitivity. Lately, a few publications have shown that laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) could provide similar results as INAA more quickly and at lower cost. A protocol has been developed to determine 51 elements using LA-ICP-MS and tested it on Wari period ceramics previously analyzed using INAA. We show how INAA and LA-ICP-MS analysis lead to the same conclusion in terms of sample groupings. 

Chemical preconcentration of the samples (e.g., extraction into chloroform and dithizone) was used in the past by several authors in order to determine the very low concentration of Pb in ancient Antarctic ice (6, 45, 64). Although this method gave reliable results, it needed a huge amount of sample (500-1000 g) and a long period of sample treatment with organic solvents. Another method is based on the preconcentration onto W wire loops that can be placed directly in a graphite furnace of instrument AAS for the atomisation of adsorbed metals for the analysis (44, 65). To minimise the contamination problems from the air of the laboratory the whole preconcentration procedure was carried out inside a vertical laminar flow clean bench. Detection limits of 0.01, 0.47, 0.22 and 0.24 pg/g were obtained for Cd, Cu, Pb and Zn respectively (44). These extremely low detection limits have recently enabled the concentrations of heavy metals in Antarctic ancient ice and recent snow to be determined (28, 72). 

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