Add time:07/31/2019 Source:sciencedirect.com
The dehydration process of the hydrated rhabdophane (cas 12174-41-3) LnPO4.0.667H2O (Ln = La to Dy) was thoroughly studied over the combination of in situ high resolution synchrotron powder diffraction and TGA experiments. In the case of SmPO4.0.667H2O (monoclinic, C2), a first dehydration step was identified around 80 °C leading to the formation of SmPO4.0.5H2O (Monoclinic, C2) with Z =12 and a =17.6264(1) Å, b =6.9704(1) Å, c =12.1141(1) Å, β=133.74(1) °, V =1075.33(1) Å3. In agreement with the TGA and dilatometry experiments, all the water molecules were evacuated above 220 °C yielding to the anhydrous form, which crystallizes in the hexagonal P3121 space group with a =7.0389(1) Å, c =6.3702(1) Å and V =273.34(1) Å3. This study was extended to selected LnPO4.0.667H2O samples (Ln= Nd, Gd, Eu, Dy) and the obtained results confirmed the existence of two dehydration steps before the stabilization of the anhydrous form, with the transitory formation of LnPO4.0.5H2O.
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