Multi-Scale Measurements of Neolithic Ceramics—A Methodological Comparison of Portable Energy-Dispersive XRF, Wavelength-Dispersive XRF, and Microcomputer Tomography

Abstract

Archaeometric investigation of ancient pottery with regard to their material composites allows insights into the material structures, production techniques and manufacturing processes. The applied methods depend on the classification of the pottery: some finds should remain unchanged for conservation reasons, other finds are less valuable or more common. While the first group cannot be destroyed for material analyses and the choice of analytical methods is limited, the latter can be investigated using destructive methods and thus can widen the spectrum of possible devices. Multi-element analyses of portable energy-dispersive X-ray fluorescence spectrometry (portable XRF) have become important for archaeological research, as portable XRF provides a quick overview about the chemical composition of potteries and can be used in non-destructive as well as destructive ways in addition to conventional microscopic examination and petrographic thin sections. While most portable XRF analyses of solely fracture surfaces do not provide satisfying results, portable XRF analyses on pulverized samples are a cost-efficient and fast alternative to wavelength-dispersive XRF (WD-XRF). In comparison to WD-XRF, portable XRF on pulverized samples provides reliable concentration data (K, Fe, Rb, Ti, V, Y, Zn, Zr), but other elements need to be corrected. X-ray microtomography (µCT) has proven to be a non-destructive technique to derive not only the porosity of ancient pottery but also to characterize temper components and non-plastic inclusions. Hence, the µCT technique has the potential to extract valuable information needed by archaeologists, for example, to deduce details about manufacturing.

Quartzite Complexities: Non-Destructive Analysis of Bifacial Points from Västerbotten, Sweden

“…Not everyone will have the benefit of working with all three instrumentations however, and in such situations XRF seems to provide more utility. Although WD-XRF systems will provide higher spectral resolution and element detection (Menne et al, 2020), portable ED-XRF has come a long way since its introduction, and instruments are becoming commonly available in archaeological laboratories.…”

“…The reference calibration used for element quantification was mining mode (Knight et al, 2021: 2), with standardised reference samples provided by the instrument supplier. The integration time was set to 130 s. Higher spectral resolution can be achieved using a Wavelength Dispersive (WD) XRF system (Menne et al, 2020). However, these systems are limited to lab-based environments and not applicable in the field, and thus not an option for the current study.…”

A review of laboratory, commercially available, and facility based wavelength dispersive X-ray fluorescence spectrometers

“…A between-bottle homogeneity test of certified reference materials investigated by Idris et al 49 was performed using the Magix PW 2403 (Malvern Panalytical, The Netherlands) wavelength dispersive instrument in a vacuum sample environment. Menne et al 50 used a MagixPRO (Malvern Panalytical) instrument to investigate ancient Neolithic pottery and to determine the elemental composition. Together with the WD-XRF technique, a portable ED-XRF instrument was used and the samples were also investigated by computed microtomography, allowing for detailed analytical comparison.…”

Using X‐ray fluorescence to examine ancient Maya granite ground stone in Belize

“…Recent advances in field‐capable portable X‐ray fluorescence (often referred to as pXRF) instrumentation have increased efficacy and suitability for archaeological sourcing studies (Barbera et al, 2013; Craig et al, 2007; Forster & Grave, 2013; Goodale et al, 2012; Menne et al, 2020). Although they are implemented in different environments, field‐based (using a portable XRF instrument) and laboratory‐based (using a larger, stationary instrument) XRF techniques operate under the same principles: an analyst uses an X‐ray beam to excite the atoms in minerals present at or near the surface of an artifact.…”

“…Our portable instrument utilizes polarized energy dispersive (ED) XRF (see Gauthier & Burke, 2011; Guthrie & Ferguson, 2012 for a full discussion of the pros and cons of each; see also e.g., Hermes & Ritchie, 1997; Lundblad et al, 2008; Williams‐Thorpe, Philip, et al, 1999). The primary advantages of field‐based XRF to archaeologists are its rapid analysis time, its nondestructive nature, and its ability to be used in the field, museum, or lab setting (e.g., Menne et al, 2020, p. 1). One instrument that can be used in a variety of settings presents a considerable saving in cost and time for training and maintenance.…”