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Investigation of multi-layered silicate ceramics using laser ablation optical emission spectrometry, laser ablation inductively coupled plasma mass spectrometry, and electron microprobe analysis

Linda Zaoralkova, Ales Hrdlicka, Vitezslav Otruba, Petr Sulovsky, Nicole Gilon, Detlef Günther, and Viktor Kanicky

Laboratory of Atomic Spectrochemistry, Department of Chemistry, Masaryk University, Brno, Kotlářská 2, CZ 611 37 Brno, Czech Republic



Abstract: The applicability of laser ablation (LA) inductively coupled plasma (ICP) spectrometry for assessing elemental distributions in layered ceramics was investigated and compared with electron probe microanalysis (EPMA). Ordinary glazed wall tiles were employed as model specimens due to their defined structure and composition. They were used for calibration in the analysis of ancient pottery. A qualitative depth profile was acquired by single-spot laser drilling perpendicular to coatings with a Nd:YAG (1064 nm) laser coupled with an ICP optical emission spectrometer (OES). The lower lateral resolution associated with the laser spot diameter of 1.0 mm led to smoothing of the depth profile due to the averaging of local irregularities. In addition, transverse line scans by ablation across the tile section using an ArF* (193 nm) laser coupled with an ICP mass spectrometer (MS) were performed. LA-ICP-OES depth profiles and LA-ICP-MS transverse scans were validated by EPMA section scans and 2D back-scattered electrons images. The LA-ICP-OES acquisition was less dependent on sample surface and layer irregularities, whereas the transverse line scan over the tile section with the small-spot beam offered insight into the micromorphology of the individual layer. The combined approach revealed the occurrence of individual mineral grains, micro-heterogeneities and the character of interfaces between layers.

Keywords: depth profile – surface analysis – inductively coupled plasma mass spectrometry – inductively coupled plasma optical spectrometry – laser ablation – electron probe X-ray microanalysis – layered ceramics

Full paper is available at

DOI: 10.2478/s11696-011-0085-3


Chemical Papers 65 (6) 769–781 (2011)

Monday, May 27, 2024

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