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

Abstract

International audienceThe 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 layer

Feasibility of Nanoparticle-Enhanced Laser Ablation Inductively Coupled Plasma Mass Spectrometry

“…4 mm, length 1 m) to the ICPMS system. For minor elements (isotopes 208 Pb, 63 Cu, 26 Mg, and 57 Fe), the dwell time per isotope was adjusted to 0.1 s and for major elements (isotopes 27 Al and 107 Ag) to 0.01 s. The total length of one cycle was then 0.246 s. Laser ablation was performed with a New Wave UP 213 system (New Wave Research, Fremont, CA) equipped with a frequencyquintupled pulsed Nd:YAG laser emitting a wavelength of 213 nm at a pulse duration of 4.2 ns fwhm with a flat-top beam profile and a helium-flushed xyz movable supercell. We chose an ablation spot of 100 μm diameter to ensure a sufficient isotopic signal and a representative area containing NPs on the sample surface.…”

“…Other materials has been tested to study the effects of the physical properties on the signal enhancement: alloy AW 6082, Al (97 wt %), Cu (<0.1 wt %), Pb (<0.003 wt %), Mg (0.9 wt %), Mn (0.7 wt %), Si (1.0 wt %), and Fe (0.1 wt %); brass MBH, Cu (62.1 wt %), Zn (35.3 wt %), Pb (1.3 wt %), Al (0.4 wt %), Fe (0.3 wt %), and Ni (0.3 wt %); certified glass standard reference material (SRM) NIST 610 as commonly used material for LA-ICPMS calibration; ceramic glaze tile L600 (Keramika HOB in Horni Briza, Czech Republic, as a subsidiary of Lasselsberger Co.). 27 Two types of spherical nanoparticles (Ag and Au) in two sizes (20 and 40 nm) were used (citrate, NanoXact, Nanocomposix, United States; mass concentration for Ag ∼30 ng mL −1 and for Au ∼50 ng mL −1 ).…”

Improvements in the direct analysis of advanced materials using ICP-based measurement techniques

“…In combination with ICP-OES, lasers with varying wavelengths showed to offer excellent depth proling capabilities as demonstrated by Kanicky et al for tungsten carbide 106 and metal-zirconia ceramic layers 107 (266 nm Nd:YAG) as well as Zr-and Ti-based nitride layers 108 (355 nm Nd:YAG). Zaoralkova et al 109 reported depth proling using 1064 nm Nd:YAG instrumentation alongside with LA-ICP-MS linescan measurements on layered silicate ceramics. An application oriented question has been presented by Michalska et al: 110 they investigated the stability of ion-selective electrodes by LA-ICP-MS depth proling.…”

Atomic spectrometry update. Industrial analysis: metals, chemicals and advanced materials

“…The systems were tested on both glass and ceramic objects, with validation achieved by using the NIST SRMs 610 glass and SRM 679 brick clay in the form of a pressed pellet. The technique of LA-ICP-MS was also used by Zaoralkova et al 294 (along with LA-ICP-OES and EPMA) to investigate multi-layered silicate ceramics. Single spot laser drilling using a Nd; YAG laser operating at 1064 nm gave a spot diameter of 1 mm.…”