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A temperature-controlled sample stage for in situ micro-X-ray diffraction; application to Mars analog mirabilite-bearing perennial cold spring precipitate mineralogy

Michael S. Bramble, Roberta L. Flemming, Jeffrey L. Hutter, Melissa M. Battler, Gordon R. Osinski and Neil R. Banerjee
A temperature-controlled sample stage for in situ micro-X-ray diffraction; application to Mars analog mirabilite-bearing perennial cold spring precipitate mineralogy
American Mineralogist (May 2014) 99 (5-6): 943-947

Abstract

A temperature-controlled sample stage with an operational range of approximately 60 degrees C above or below ambient laboratory temperature (approximately -35 to 85 degrees C) was constructed for in situ X-ray diffraction of minerals and materials using a Bruker D8 Discover diffractometer with theta -theta geometry. The stage was primarily designed for characterizing mirabilite-bearing samples from a Mars analog High Arctic perennial cold spring at an in situ temperature. Operation of the stage was demonstrated through the analysis of a synthetic sample of the hydrated sodium sulfate, mirabilite (Na (sub 2) SO (sub 4) .10H (sub 2) O). Mirabilite was held at -25 degrees C for approximately two hours without significant dehydration and then incrementally warmed to ambient laboratory temperature at 5 degrees C intervals, during the acquisition of in situ diffraction data. At ambient laboratory temperature, the mirabilite dehydrated and only polycrystalline thenardite (Na (sub 2) SO (sub 4) ) remained. Preliminary analysis of the cold spring precipitates demonstrates that when mirabilite is present in the sample the dehydration reaction is occurring between collection and analysis at ambient laboratory temperature. This temperature-controlled stage was designed for versatility and ease of X-ray access, with applications that can extend to many geological and planetary settings, including Mars analog environments.


ISSN: 0003-004X
EISSN: 1945-3027
Coden: AMMIAY
Serial Title: American Mineralogist
Serial Volume: 99
Serial Issue: 5-6
Title: A temperature-controlled sample stage for in situ micro-X-ray diffraction; application to Mars analog mirabilite-bearing perennial cold spring precipitate mineralogy
Affiliation: University of Western Ontario, Centre for Planetary Science and Exploration, London, ON, Canada
Pages: 943-947
Published: 201405
Text Language: English
Publisher: Mineralogical Society of America, Washington, DC, United States
References: 12
Accession Number: 2014-048817
Categories: Mineralogy of non-silicatesExtraterrestrial geology
Document Type: Serial
Bibliographic Level: Analytic
Illustration Description: illus.
Country of Publication: United States
Secondary Affiliation: GeoRef, Copyright 2017, American Geosciences Institute. Abstract, copyright, Mineralogical Society of America. Reference includes data from GeoScienceWorld, Alexandria, VA, United States
Update Code: 201427
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