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The radiation effect of luminescence emission of Ca‐rich oxalate biogenic materials (gallbladder and renal calculi) and a commercial standard sample (CaC2O4·H2O) is reported. The samples were characterized by environmental scanning electron microscopy, energy dispersive X‐ray spectroscopy, thermogravimetric and differential thermal analyses, display complex cathodoluminescence (CL) and thermoluminescence (TL) glow emissions. CL spectra (in the UV−infrared range) displayed non‐well defined peaks, and exhibited emission at: (i) higher energies (300–490 nm) mainly associated with non‐bridging oxygen hole centers, oxygen‐deficient centers and peroxy intrinsic defects, regardless of the sample; and (ii) higher, narrow and sharp wavebands, in the red region, probably induced by the presence of traces of Sm3+ (4G5/2→6H9/2 transition) and/or Tb3+ (5D4→7F3 transition) only for mineral‐like materials in the human body. The UV‐blue TL emission showed low‐intensity maxima in which it was possible to distinguish at least four groups of components in each sample.