Investigation of high-pressure planetary ices by cryo-recovery. II. High-pressure apparatus, examples and a new high-pressure phase of MgSO4·5H2O

An apparatus is described for the compression of samples to ∼2 GPa at temperatures from 80 to 300 K, rapid chilling to 80 K whilst under load and subsequent recovery into liquid nitro-gen after the load is released. In this way, a variety of quenchable high-pressure phases of many materials may be p...

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Veröffentlicht in:Journal of applied crystallography. - 1998. - 51(2018), Pt 3 vom: 01. Juni, Seite 692-705
1. Verfasser: Wang, Weiwei (VerfasserIn)
Weitere Verfasser: Fortes, A Dominic, Dobson, David P, Howard, Christopher M, Bowles, John, Hughes, Neil J, Wood, Ian G
Format: Online-Aufsatz
Sprache:English
Veröffentlicht: 2018
Zugriff auf das übergeordnete Werk:Journal of applied crystallography
Schlagworte:Journal Article cryo-recovery epsomite high pressure magnesium sulfate pentahydrate planetary ices
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520 |a An apparatus is described for the compression of samples to ∼2 GPa at temperatures from 80 to 300 K, rapid chilling to 80 K whilst under load and subsequent recovery into liquid nitro-gen after the load is released. In this way, a variety of quenchable high-pressure phases of many materials may be preserved for examination outside the high-pressure sample environment, with the principal benefit being the ability to obtain high-resolution powder diffraction data for phase identification and structure solution. The use of this apparatus, in combination with a newly developed cold-loadable low-temperature stage for X-ray powder diffraction (the PheniX-FL), is illustrated using ice VI (a high-pressure polymorph of ordinary water ice that is thermodynamically stable only above ∼0.6 GPa) as an example. A second example using synthetic epsomite (MgSO4·7H2O) reveals that, at ∼1.6 GPa and 293 K, it undergoes incongruent melting to form MgSO4·5H2O plus brine, contributing to a long-standing debate on the nature of the high-pressure behaviour of this and similar highly hydrated materials. The crystal structure of this new high-pressure polymorph of MgSO4·5H2O has been determined at 85 K in space group Pna21 from the X-ray powder diffraction pattern of a sample recovered into liquid nitro-gen and is found to differ from that of the known ambient-pressure phase of MgSO4·5H2O (pentahydrite, space group ), consisting of corner-sharing MgO6-SO4 ion pairs rather than infinite corner-sharing chains 
650 4 |a Journal Article 
650 4 |a cryo-recovery 
650 4 |a epsomite 
650 4 |a high pressure 
650 4 |a magnesium sulfate pentahydrate 
650 4 |a planetary ices 
700 1 |a Fortes, A Dominic  |e verfasserin  |4 aut 
700 1 |a Dobson, David P  |e verfasserin  |4 aut 
700 1 |a Howard, Christopher M  |e verfasserin  |4 aut 
700 1 |a Bowles, John  |e verfasserin  |4 aut 
700 1 |a Hughes, Neil J  |e verfasserin  |4 aut 
700 1 |a Wood, Ian G  |e verfasserin  |4 aut 
773 0 8 |i Enthalten in  |t Journal of applied crystallography  |d 1998  |g 51(2018), Pt 3 vom: 01. Juni, Seite 692-705  |w (DE-627)NLM098121561  |x 0021-8898  |7 nnns 
773 1 8 |g volume:51  |g year:2018  |g number:Pt 3  |g day:01  |g month:06  |g pages:692-705 
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