Homogeneity testing and quantitative analysis of manganese (Mn) in vitrified Mn-doped glasses by laser-induced breakdown spectroscopy (LIBS)

Abstract

Laser-induced breakdown spectroscopy (LIBS), an atomic emission spectroscopy method, has rapidly grown as one of the best elemental analysis techniques over the past two decades. Homogeneity testing and quantitative analysis of manganese (Mn) in manganese-doped glasses have been carried out using an optimized LIBS system employing a nanosecond ultraviolet Nd:YAG laser as the source of excitation. The glass samples have been prepared using conventional vitrification methods. The laser pulse irradiance on the surface of the glass samples placed in air at atmospheric pressure was about 1.7×109 W/cm2. The spatially integrated plasma emission was collected and imaged on to the spectrograph slit using an optical-fiber-based collection system. Homogeneity was checked by recording LIBS spectra from different sites on the sample surface and analyzing the elemental emission intensities for concentration determination. Validation of the observed LIBS results was done by comparison with scanning electron microscope- energy dispersive X-ray spectroscopy (SEM-EDX) surface elemental mapping. The analytical performance of the LIBS system has been evaluated through the correlation of the LIBS determined concentrations of Mn with its certified values. The results are found to be in very good agreement with the certified concentrations.

Assessing glass‐ceramic homogeneity and nucleation self‐correlation by crystallization statistics

“…To access the chemical homogeneity of glasses, optical 1–4 and chemical 5,6 procedures have been proposed. However, since all these methods have some limitations, chemical homogeneity determination is still a current challenge.…”

“…However, since all these methods have some limitations, chemical homogeneity determination is still a current challenge. Such limitations include inconsistent results of optical methods based on the Christiansen‐Shelyubskii procedure, 7,8 and the difficulty in obtaining, interpreting, and getting an accurate estimate of the elemental composition due to the considerable amount of spectra generated by chemical methods, 9 such as laser‐induced breakdown spectroscopy (LIBS) 5 and laser ablation inductively coupled plasma mass spectrometry (LA‐ICP‐MS) 6 . Even though these chemical methods could determine if a given glass is homogeneous, the lowest spatial scale is limited by the laser spot size, generally of several microns.…”