A multi-methodological study, based on electron microprobe analysis (in wavelength dispersive mode), single-crystal X-ray diffraction (XRD), transmission electron microscopy and single-crystal Fourier transform infrared spectroscopy was performed in order to describe the crystal chemistry of four leucite samples from different localities of the Roman Comagmatic Province (central Italy). All the crystals examined were found to be tetragonal (space group I41/a with a = 13.076–13.103 Å and c = 13.744–13.784 Å) and characterized by a complex twinning (merohedric twins: on the tetragonal planes (110) and (1̄10) with the two individuals having parallel crystallographic axes with a and b interchanged; pseudo-merohedric twins: on the tetragonal planes (101), (011), (1̄01), (01̄ 1), with the two individuals having parallel a (or b) axes and the remaining two axes not parallel). The chemical analyses show that all the samples contain minor Na and Fe. Infrared spectroscopy shows that all samples contain structurally bound water molecules, up to unexpectedly large amounts (~0.4 wt.%) for a nominally anhydrous mineral, suggesting that ‘analcime-like’ substitution (K to Na + H2O) occurs in the leucite samples investigated here. The detection limits of the ‘analcime-like’ substitution by singlecrystal XRD are also discussed.

A multi-methodological investigation of a synthetic Cu/Fe-bearing blue beryl [IV(Be2.86Cu0.14)∑=3.00VI(Al1.83Fe3+0.14Mn2+0.03Mg0.03)∑=2.03IV(Si5.97Al0.03∑=6.00O18.(Li0.12Na0.04.0.40H2O)] has been performed by means of gemmological standard testing, electron microprobe chemical analyses, laser ablation inductively coupled plasma mass spectroscopy, thermo-gravimetric analyses, infrared spectroscopy and single-crystal X-ray diffraction in order to determine the gemmological properties, crystal structure and crystal-chemistry of this material. The increasing production of marketable hydrothermal synthetic beryls with 'exotic' colours and the small number of studies on the accurate location of chromophores in the crystal structure inspired this multi-methodological investigation. The X-ray structural refinements confirm that the space group of the Cu/Fe-bearing blue beryl is P6/mcc, with unit-cell parameters: 9.2483 ≤ a ≤ 9.2502 Å and 9.2184 ≤ c ≤ 9.2211 Å. The analysis of the difference Fourier maps of the electron density suggests that Cu is located at the tetrahedral site (Wyckoff 6fposition) along with Be, whereas Fe shares the octahedral site with Al (4c position). No evidence of extra-framework Cu/Fe-sites (i.e. channel sites) has been found. The Li is probably located at the extra-framework 2b site. Infrared spectra show that the H2O molecules are present with two configurations: one with the H···H vector oriented ‖[0001] and the other with H···H vector oriented ⊥[0001].