Electron energy-loss spectroscopy and electron probe X-ray microanalysis of exhaust aerosols in slurry nebulization inductively coupled plasma atomic spectrometry for ceramic powders

Abstract

Exhaust aerosols in inductively coupled plasma (ICP) atomic spectrometry generated from different ceramic powder suspensions (Al 2O 3, ZrO 2 and SiC) were investigated by electron energy loss spectroscopy (EELS) and electron probe X-ray micro analysis (EPXMA). Differences in morphology, size and elemental composition of sub-micrometer residues of these refractory powders, collected above ICPs operated with different gasses, were found to depend on the outer gas (N 2 O 2 and Ar), the distance between the impacting stage and the plasma, and on the ceramic powder introduced as a slurry into a suitable nebulizer. Identical exhaust types of particles were observed in the case of Al 2O 2 and ZrO 2 slurries, also when different outer gases and different operation conditions were used. For SiC, much depends on the outer gas used, as shown by morphological and chemical composition studies. Electron energy loss spectroscopy and element spectroscopic imaging (ESI) were used for the elemental analysis and the localization of the detected elements (Al, Zr, Si, C, O and N) in the individual exhaust particles.