A light REE (LREE)-bearing mineral called chevkinite (Ce, La, Ca, Th)4(Fe2+, Mg)2(Ti, Fe3+)3Si4O22, originating from a heavy metal placer deposit Aksu Diamas in Turkey, previously assessed for potential REE extraction as a by-product of magnetite production, was studied using scanning electron microscopy with energy and wavelength-dispersive spectrometers (SEM EDS-WDS). This mineral exhibits analytical challenges associated with severe X-ray energy overlaps between the REE, titanium, and barium. Here, we present an iterative process, showing that SEM EDS-WDS is a viable technique for obtaining good quality quantitative data. SEM EDS-WDS is an in situ, non-destructive, and relatively non-expensive technique, but operator’s experience is essential to obtain good quality data. In cases where the peak fitting remains challenging, in particular, and where the constituents have large differences in abundance, an assessment of the X-ray spectrum to qualitatively assign all peaks is essential prior to quantitative analysis.