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Spectroscopic measurements of flames are amongst the most important analytical diagnostic techniques that allow one to improve thermal and energy efficiency of industrial furnaces. A chemical seeding laser-induced plasma spectroscopy (CS-LIPS) was successfully developed and applied for mixing analysis of a methane–air diffusion flame. The results obtained showed that sensitivity of this system was much improved using silica rod as the target material in place of the tungsten material used in our previous studies. Profiling of Mg spectral emission and mixing in the flame was made more clearly with the introduction of magnesium aerosols as a tracer into the combustion air flow.