The goal of accurately quantifying trace elements in ultrapure silicon carbide (SiC) with a purity target of 5N (99.999% purity) was addressed. The unsuitability of microwave-assisted acid digestion followed by Inductively Coupled Plasma Mass Spectrometry (ICP-MS) analysis was proved to depend mainly on the contamination induced by memory effects of PTFE microwave vessels and by the purity levels of acids, even if highly pure ones were used in a clean environment. A new analytical protocol for the direct analysis of the solid material by laser ablation coupled with ICP-MS (LA-ICP-MS) was then exploited. Different samples were studied; the best results were obtained by embedding SiC (powders or grains) in epoxy resin. This technique has the great advantage of avoiding any source of external contamination, as grinding, pressing and sintering pretreatments are totally unnecessary. Two different laser wavelengths (266 and 193 nm) were tested, and best results were obtained with the 266 nm laser. The optimized protocol allows the determination of elements down to the sub-mg/kg level with a good accuracy level.

Tackling the Challenging Determination of Trace Elements in Ultrapure Silicon Carbide by LA-ICP-MS

Spanu, Davide
Primo
;
Palestra, Alessandro;Prina, Veronica;Monticelli, Damiano;Bonanomi, Simone;Binda, Gilberto;Rampazzi, Laura;Recchia, Sandro
Ultimo
2023-01-01

Abstract

The goal of accurately quantifying trace elements in ultrapure silicon carbide (SiC) with a purity target of 5N (99.999% purity) was addressed. The unsuitability of microwave-assisted acid digestion followed by Inductively Coupled Plasma Mass Spectrometry (ICP-MS) analysis was proved to depend mainly on the contamination induced by memory effects of PTFE microwave vessels and by the purity levels of acids, even if highly pure ones were used in a clean environment. A new analytical protocol for the direct analysis of the solid material by laser ablation coupled with ICP-MS (LA-ICP-MS) was then exploited. Different samples were studied; the best results were obtained by embedding SiC (powders or grains) in epoxy resin. This technique has the great advantage of avoiding any source of external contamination, as grinding, pressing and sintering pretreatments are totally unnecessary. Two different laser wavelengths (266 and 193 nm) were tested, and best results were obtained with the 266 nm laser. The optimized protocol allows the determination of elements down to the sub-mg/kg level with a good accuracy level.
2023
2023
ICP-MS; LA-ICP-MS; direct analysis; laser ablation; microwave-assisted acid digestion; silicon carbide; trace elements
Spanu, Davide; Palestra, Alessandro; Prina, Veronica; Monticelli, Damiano; Bonanomi, Simone; Nanot, Sandro Usseglio; Binda, Gilberto; Rampazzi, Laura; Sessa, Gianluca; Callejo Munoz, David; Recchia, Sandro
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Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/11383/2151112
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