A neutron powder diffraction study of the phases in solid D3O·ClO4

Domosl̄awski, J.; Gołąb, Małgorzata

doi:10.1016/0378-4363(80)90105-9

Cited by 4 publications

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“…The presence of two phases for H30+C1C>4~h as been confirmed by adiabatic calorimetry,8 but a third intermediate phase occurring over a very short temperature range was suggested by the results for the deuteriated material D30+C1C>4~.9 Curiously, powder diffraction studies on this intermediate phase showed very little difference between this and the lowtemperature phase. 7 NMR studies have appeared frequently (see ref 2). Early NMR line shape studies of perchloric acid monohydrate were the first experiments to unequivocally establish the existence of an oxonium ion H30+ as a stable entity,10•11 and the H-H distance was determined to be 1.70 Á. line shapes, second moments (M2), and spin-lattice relaxation times 7¡ and T\e as a function of temperature12 showed the onset of reorientation about the 3-fold axis of the ion in the low-temperature phase, with an activation energy of £a = 20.2 kJ/mol.…”

Section: Introductionmentioning

confidence: 99%

A 2H NMR Study of the Phases and Motions in Solid Oxonium Perchlorate, D3O+ClO4-

Ratcliffe¹

1994

J. Phys. Chem.

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2H NMR has been used to reexamine and clarify the phase behavior and molecular motions in solid D@+C104-.In the low-temperature phase reorientation about the molecular 3-fold axis of the D30+ ion is confirmed.The NMR results above 200 K, together with calorimetric data, show some dramatic effects due to eutectic behavior arising from small quantities of water in excess of the monohydrate stoichiometry. The true phases of D@'C104-have now been identified; only one solid-solid phase transition occurs, with hysteresis, at 245 K on cooling and 254 K on warming. Motion in the room temperature phase is not isotropic. Isotropic lines reported earlier presumably were due to the molten eutectic mixture.

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Section: Introductionmentioning

confidence: 99%