Synchrotron-based XRD has been applied to shells. Investigation of crystallographic phase composition. Understanding of structures at molecular level. SEM to explore the morphology of the snail and bivalve. Extraction of the lattice parameters of the mineral CaCO 3 . a r t i c l e i n f o a b s t r a c tSynchrotron-based high-resolution X-ray powder diffraction spectra from the body parts of a snail and bivalve (CaCO 3 ), have been recorded with Pilatus area detector. Experiments were performed at Desy, Hamburg, Germany, utilizing the Resonant and Diffraction beamline (P9), with 15 keV X-rays (λ ¼0.82666 Å). The external shell of these living organisms, is composed of calcium carbonate, which carries strong biological signal. It consists of some light elements, such as, Ca, C and O, which constitute part of the soft tissue and other trace elements. The knowledge of these diffraction patterns and hence the understanding of structures at molecular level are enormous. The application of synchrotron radiation to powder diffraction is well suited for samples of biological nature via changes in their patterns and also to investigate crystallographic phase composition. With the use of Rietveld refinement procedure, to the high-resolution diffraction spectra, we were able to extract the lattice parameters of orthorhombic polymorph of CaCO 3 , the most abundant mineral produced by these living organisms. The small size of the crystallite is a very important factor related to the biological structure. The natural model presents a combination of organic and inorganic phases with nanometer size. For the present study, we also used the scanning electron microscopy (SEM) to explore the associated morphology of the snail and bivalve.