Hydrate Layers on Ice Particles and Superheated Ice: A 1H NMR Microimaging Study 1

Journal of Physical Chemistry A

Volumn 103, Issue 26, 1999, Pages

  Moudrakovski, Igor L ^a   Ratcliffe, Christopher I ^a   McLaurin, Graham E ^a   Simard, Benoit ^a   Ripmeester, John A ^a  

^a NATIONAL RESEARCH COUNCIL CANADA   (Canada)

Author keywords

[No Author keywords available]

Indexed keywords

EID: 0042133083     PISSN: 10895639     EISSN: None     Source Type: Journal    
DOI: None     Document Type: Article

References (31)

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20. 2/g.
21. Moudrakovski, I. L.; Sanchez, A.; Ratcliffe, C. I.; MacLaurin, G. E.; Simard, B.; Ripmeester, J. A., to be published.
22. Before measurement, each sample was kept at 273 K for 15-18 h and for 1.5 h at each temperature of measurement.
23. The temperature gradient in the probe was estimated from multislice images of the melting process of ice in a bundle of 16 glass capillaries.
24. Gas uptake experiments were carried out in a cylindrical high- pressure cell in which the gas pressure could be controlled by adjusting a precision gas injector. Circulating fluid from a programmable temperature bath controlled the temperature. The cell was loaded with ice (≈5 g) inside a freezer at ≈250 K, evacuated to remove air, pressurized with methane gas, and connected to the circulating bath. The gas injector was adjusted to keep the pressure inside the cell constant as methane was consumed in the conversion to hydrate, and gas uptake was measured from the position of the gas injector piston.
25. The hydrate and ice Ih structures are incommensurate, and hence there should be an interface that is disorganized, if not liquid, at temperatures near the melting point of ice. We note also the evidence for melting at grain boundaries below the bulk melting point in polycrystalline ice: Salvetti, G.; Tombari, E.; Johari, G. P. J. Chem. Phys. 1995, 102, 4987. Internal melting at imperfections in single crystals of ice: Gagnon, R. E.; Tulk, C.; Kiefte, H. J. Glaciology 1994, 40, 132.
26. The hydrate and ice Ih structures are incommensurate, and hence there should be an interface that is disorganized, if not liquid, at temperatures near the melting point of ice. We note also the evidence for melting at grain boundaries below the bulk melting point in polycrystalline ice: Salvetti, G.; Tombari, E.; Johari, G. P. J. Chem. Phys. 1995, 102, 4987. Internal melting at imperfections in single crystals of ice: Gagnon, R. E.; Tulk, C.; Kiefte, H. J. Glaciology 1994, 40, 132.
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30. For most samples, the pressures reported are actual equilibrium pressures. These were measured by comparing the intensity of the methane gas proton signal in a 1-mm image slice above the ice and a reference sample. For the 119 bar sample, the pressure reported was the initial pressure; since the amount of gas in the tube far exceeds that consumed during the reaction, the pressure change is ≈12% during conversion to hydrate.
31. Callaghan, P. T. Principles of Nuclear Magnetic Resonance Microscopy; Oxford University Press: Oxford, 1991.