Spectrochimica Acta Part B: Atomic Spectroscopy

This work investigates the analytical possibilities of high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS) for the direct determination of Pd, Pt and Rh (PGMs) in spent automobile catalysts. A novel approach for the microwave dissolution with the mixture of HCl and H2O2 (4:1) was developed for the further HR CS GFAAS. It was found that within 20 minutes at the temperature 210°C of the PGMs quantitatively and simultaneously transferred to solution. It did not show any matrix interferences in determining Pd and Rh, when using HR CS GFAAS for determining the PGMs. When determining Pt, the matrix effect can be expressly minimized by diluting the sample or applying a corrective model. Limits of quantification (μg L-1) by HR CS GFAAS achieved were 1 (Pd), 2 (Pt), and 0.5 (Rh). Correlation coefficients were 0.9973 (Pd), 0.9995 (Pt), and 0.9983 (Rh). The relative standards deviation for PGM determination by the developed procedure was not higher than 5 % in the concentration range 0.0005-0.5 % weight. Moreover, validation of the process of evaluation of metrological characteristics for the sample preparation method developed in this research, demonstrated that it is resistant to changes in the samples of spent automobile catalysts. The correctness of experimental results was assured by the optical emission with inductively coupled plasma method comparisons.

Averaged LIBS spectra of emeralds and steel coupons used in this study.

This file contains the Gaussian fitting results of the obtained spectra. And it also gives the caculated values of the high-lying excited states.

Raw data for Arctic sediments measured by LIBS, XRF, and ICP.

The present work aims to evaluate the alteration conditions of historical limestone rocks exposed to urban environment using the Laser-Induced Breakdown Spectroscopy (LIBS) technique. The approach proposed is based on the microscale three dimensional (3D) compositional imaging of the sample through double-pulse micro-Laser-Induced Breakdown Spectroscopy (DP-μLIBS) in conjunction with optical microscopy. DP-μLIBS allows to perform a quick and detailed in-depth analysis of the composition of the weathered artifact by creating a ‘virtual thin section’ (VTS) of the sample which can estimate the extent of the alteration processes occurred at the limestone surface. The DP-μLIBS analysis of these thin sections showed a reduction with depth of the elements (mainly Fe, Si and Na) originating from atmospheric dust, particulate deposition and the surrounding environment (due to the proximity of the sea), whereas, the LIBS signal of Ca increased in intensity from the black crust to the limestone underneath.