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This paper provides a comprehensive assessment of the Kenticha pegmatite-spodumene ore, specifically evaluating its potential to yield Li, Nb, and Ta using advanced spectroscopic techniques such as ToF-ERDA, PIXE, EDS, and XRD. The samples were categorized into three subsamples (KS1, KS2, KS3) based on color, texture, density, and lithology, as well as two additional samples (KS4 and KS5) based on their magnetic response. XRD patterns confirmed the predominance of spodumene, along with lesser amounts of silica oxide, albite, muscovite, magnetite, kaolinite, silicon oxide, iron silicide, and lithium iron oxide in samples KN, KS1, KS2, and KS3. The dominant phases in samples KS4 and KS5 were identified as manganocolumbite, ferrocolumbite, ferrous niobate, and manganese alumina oxide. Importantly, ToF-ERDA analysis revealed that samples KN, KS1, KS2, and KS3 contained H, Li, Be, C, N, O, Na, Al, Si, K, and Fe. In addition, samples KS4 and KS5 exhibited Na, Ta, and U. Sample KS2 displayed the highest weight percent (wt%) concentrations of Li, Be, C, O, F, Na, Si, and K, with an impressive Li content of 0.096 wt%, significantly higher compared to 0.036, 0.066, and 0.047 wt% found in samples KN, KS1, and KS3, respectively. Furthermore, ToF-ERDA indicated that the non-magnetic sample KS4 had elevated wt% of Mn at 0.736, Nb at 28.59, and Ta at 12.11, whereas the magnetic sample KS5 showed lower wt% for Li (0.041) and Fe (27.006). Meanwhile, the PIXE analysis revealed significant at% concentrations of Cr, Mn, Fe, Ni, Zn, Ga, Rb, Nb, In, Ta, Th, and U among 76 elements. Compared to KN, KS1, and KS3, the sample KS2 displayed higher wt% of Mn, Ni, Zn, Ga, In, and Th, while exhibiting lower levels of Fe, Nb, and Ta. SEM–EDS spectra indicated higher at% averages of O, Fe, Al, and Si in samples, following the order KS2 > KS3 > KN > KS1, indicative of aluminosilicates. Gravity and magnetic separation of the pegmatite-spodumene ore yielded manganocolumbite (KS4), which contains 28.59 wt% Nb and 12.11 wt% Ta, distinct from the magnetic ferocolumbite (KS5). These findings underscore the potential for increased extraction and utilization of Li, Nb, and Ta in applications such as lithium-ion batteries, fuel cells, and nuclear reactors.