A new device to mount portable energy-dispersive X-ray fluorescence spectrometers (p-ED-XRF) for semi-continuous analyses of split (sediment) cores and solid samples

Abstract

Abstract. Portable energy-dispersive X-ray fluorescence spectrometers (p-ED-XRF) have become increasingly popular in sedimentary laboratories to quantify the chemical composition of a range of materials such as sediments, soils, solid samples, and artefacts. Here, we introduce a low-cost, clearly arranged unit that functions as a sample chamber (German industrial property rights no. 20 2014 106 048.0) for p-ED-XRF devices to facilitate economic, non-destructive, fast, and semi-continuous analysis of (sediment) cores or other solid samples. The spatial resolution of the measurements is limited to the specifications of the applied p-ED-XRF device – in our case a Thermo Scientific Niton XL3t p-ED-XRF spectrometer with a maximum spatial resolution of 0.3 cm and equipped with a charge-coupled device (CCD) camera to document the measurement spot. We demonstrate the strength of combining p-ED-XRF analyses with this new sample chamber to identify Holocene facies changes (e.g. marine vs. terrestrial sedimentary facies) using a sediment core from an estuarine environment in the context of a geoarchaeological investigation at the Atlantic coast of southern Spain.

Quantitative micro‐X‐ray fluorescence scanning spectroscopy of wet sediment based on the X‐ray absorption and emission theories: Its application to freshwater lake sedimentary sequences

“…It is not mandatory to use μ ‐XRF scanning spectroscopy equipped to perform X‐ray radiography, such as scanning X‐ray analytical microscope (SXAM) and Itrax‐XRF core loggers (Croudace et al ., ). For example, on the one hand μ ‐XRF intensities can be measured with the Avaatech XRF core scanner (Richter et al ., ) and the XRF handheld spectrometers (Hoelzmann et al ., ), and on the other hand linear absorption coefficients of wet sediments can be calibrated with an X‐ray computed tomography scanner (Oda et al ., ) and gamma ray attenuation density scanner (Best & Gunn, ). The proposed method has, therefore, the possibility to become a future standard protocol for μ ‐XRF scanning spectroscopy core‐loggers for wet sediments in combination with XRT measurements.…”

“…(), but this approach was improved upon with the following: (i) estimation of water content using XRT intensities was changed from an equation based on mass absorption coefficients to linear absorption coefficients (LAC); and (ii) the instrument's sensitivity to each element was given by an XRF correction equation. Its validity on the XRF correction was confirmed for incident X‐rays with a continuous spectral energy distribution, which is typical of the X‐ray beams commonly used in μ ‐XRF instruments and handheld spectrometers (Richter et al ., ; Hoelzmann et al ., ; Ryan et al ., ).…”

“…Reconstruction of palaeoenvironmental changes, as well as determination of depositional processes and basin architecture, through sediment analysis is one of the key components in sedimentology. During the past two decades, progress in science and technology has enabled non-destructive, automated micro-X-ray fluorescence (l-XRF) scanning spectroscopy on large numbers of split sediment core sections (see Hosokawa et al, 1997;Phedorin & Goldberg, 2005;Croudace et al, 2006;Haschke, 2006;Richter et al, 2006;Hoelzmann et al, 2017). In turn, this has enabled the rapid acquisition of high-resolution records of element intensities for marine, lacustrine and fluvial sedimentary sequences, allowing detailed palaeoenvironmental interpretations, the reliable assessment of palaeoredox conditions and the accurate identification of the genetic units (Katsuta et al, 2007;Naeher et al, 2013;Vanneste et al, 2013;Wirth et al, 2013;Costa et al, 2018).…”

Reconstructing human–landscape interactions in the context of ancient iron smelting on Elba Island, Italy, using sedimentological evidence

“…Homogenized and air‐dried samples were transferred to a sample cell and covered with a 0.4 µm polyethylene terephthalate film (BoPET; Mylar, DuPont, Wilmington, DE) and measured under standardized conditions in a sample chamber. In addition, in situ measurements of air‐dried core halves were logged semi‐continuously in an arranged unit (Hoelzmann, Klein, Kutz, & Schütt, ) with 13 mm spot size every 2 cm without a thin film. Sediment samples were measured in the standard “mining Cu/Zn” mode with main, high, low, and light filters (50, 50, 15/20, and 8 kV, respectively) with a total measurement duration of 120 s. Our results were compared with certified reference material (LKSD‐4; Lynch, ) and an acid‐purified silica sand during operation to ensure measurement quality; recoveries of major oxides range between 75% and 125% except for K (135%).…”

Environmental Changes and Cultural Transitions in SW Iberia during the Early-Mid Holocene

“…Ca/Si ratio points to the carbonated vs. siliciclastic sources [65,66], while Si/Al and Zr/Al are used as textural proxies like sorting or grain size [38,67] (Figure 4f). These ratios show no clear trends, as those mentioned before, but they can be divided in three stages: from 12 until 8.8 ka BP, their record show low amplitude cycles that shorten their period in time, Ca/Si decreases while Zr/Al and Si/Al remain, showing a slowly increasing trend; from that time until ca.…”