Abstract

In this study, a possibility of laser-induced breakdown spectroscopy (LIBS) for the analysis of zeolites containing copper, chromium, cobalt, cadmium, and lead in the concentration range of 0.05–0.5 wt.% is discussed. For the LIBS analysis, microporous ammonium form of Y zeolite with the silicon to aluminum molar ratio of 2.49 was selected. Zeolites, in the form of pressed pellets, were prepared by volume impregnation from the water solution using Co(CH3COO)2.4H2O, CuSO4.5H20, K2Cr2O7, PbNO3, and CdCl2 to form a sample with different amounts of heavy metals—Co, Cu, Cr, Pb, and Cd. Several spectral lines of the mentioned elements were selected to be fitted to obtain integral line intensity. To prevent the influence of the self-absorption effect, non-resonant spectral lines were selected for the calibration curves construction in most cases. The calibration curves of all elements are observed to be linear with high regression coefficients. On the other hand, the limits of detection (LOD) were calculated according to the 3σ/S formula using the most intensive spectral lines of individual elements, which are 14.4 ppm for copper, 18.5 ppm for cobalt, 16.4 ppm for chromium, 190.7 ppm for cadmium, and 62.6 ppm for lead.

Highlights

  • Zeolites and zeolite-like materials belong to the group of crystalline porous materials, which structure is based on the tetrahedral networks of SiO4 and AlO4 [1]

  • The most commonly used method to compensate the dependence between the calibration curves of the spectral lines and the internal standard lines with a similar value of the upper energy levels and the plasma parameters, is to normalize the spectral line intensity of the and both elements should have similar ionization energies (Table 2)

  • The influence of the electron temperature on the calibration curves was reduced by selecting of the spectral lines and the Ionization internal standard lines with a similar value of the upper energy levels and both elements Sishould have similar ionization energies (Table 2)

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Summary

Introduction

Zeolites and zeolite-like materials belong to the group of crystalline porous materials, which structure is based on the tetrahedral networks of SiO4 and AlO4 [1]. Many studies dedicated on the use of natural and synthesized zeolites for the removal of heavy metals in water, wastewater, soils, etc., have been published [5,6,7,8]. Calibration-free laser induced breakdown spectroscopy (CF LIBS) were successfully applied for the determination of Si/Al molar ratios in different zeolite types [10]. Laser-induced breakdown spectroscopy was applied for the analysis of NH4 Y zeolites, for the detection of heavy metals (Cu, Co, Cr, Cd, and Pb) in zeolite’s matrix, for the construction of calibration curves, and for the determination of the detection limits for these five heavy metals

LIBS Apparatus
Zeolite Samples Preparation
Results
Diagnostics of Laser-Induced Plasma
Influence of the the
Copper
Cadmium
Cobalt
Chromium
Limits of Detection
Conclusion
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