• Journal of the Mineralogical Society of Korea
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• v.26 no.3
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• pp.175-187
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• 2013

In-situ Raman and X-ray diffraction experiments have been performed on mineral natrolite (Na-zeolite) to investigate the dehydration behavior under high temperature and high pressure-temperature conditions. XRD data show reversible dehydration up to $450^{\circ}C$ whereas Raman data show irreversible change when the material is heated up to $630^{\circ}C$. The existence of post-natrolite was newly identified to form from ${\beta}$-metanatrolite at $380^{\circ}C$ upon cooling. The formation of dehydrated metanatrolite under simultaneous high temperature-pressure (room temperature < T < $300^{\circ}C$, 0 GPa < P < 2.1 GPa) conditions was not observed.

• Economic and Environmental Geology
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• v.45 no.2
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• pp.79-88
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• 2012

The increased brightness and focused X-ray beams now available from laboratory X-ray sources facilitates a variety of powder diffraction experiments not practical using conventional in-house sources. Furthermore, the increased availability of 2-dimensional area detectors, along with implementation of improved software and customized sample environmental cells, makes possible new classes of in-situ and time-resolved diffraction experiments. These include phase transitions under variable pressure- and temperature conditions and ion-exchange reactions. Examples of in-situ and time-resolved studies which are presented here include: (1) time-resolved data to evaluate the kinetics and mechanism of ion exchange in mineral natrolite; (2) in-situ dehydration and thermal expansion behaviors of ion-exchanged natrolite; and (3) observations of the phases forming under controlled hydrostatic pressure conditions in ion-exchanged natrolite. Both the quantity and quality of the in-situ diffraction data are such to allow evaluation of the reaction pathway and Rietveld analysis on selected dataset. These laboratory-based in-situ studies will increase the predictability of the follow-up experiments at more specialized beamlines at the synchrotron.

• Economic and Environmental Geology
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• v.56 no.1
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• pp.13-21
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• 2023

X-ray powder diffraction study was conducted on the bulk modulus and phase transition behavior of synthetic zeolite X under high temperature and high pressure. Water and HCO₃^- solution were used as a PTM. Sample was heated and pressurized up to 250 ℃ and 5.18 GPa. The change of unit cell volume and phase transition were observed by X-ray diffraction. The lattice constants and unit cell volume of zeolite X, gmelinite, natrolite, and smectite were calculated using the GSAS2 program to which Le Bail's whole powder pattern decomposition (WPPD) method was applied. The bulk modulus of each zeolite X and smectite were calculated using the EosFit program to which the Birch-Murnaghan equation was applied. The bulk modulus of zeolite X is 89(3) GPa in water run, and zeolite X is 92(3) GPa in HCO₃^- solution run. In both run, pressure induced hydration (PIH) occurred due to the inflow of PTM into the zeolite X framework at initial pressure. Zeolite X transited to gmelinite, natrolite, and smectite in water run. Zeolite X, however, transited to smectite in HCO₃^- solution run. Interzeolite transformation occurred in water run, and did not occur in HCO₃^- solution run, which is assumed that conflict between the environment to form zeolite and the pH of the HCO₃^- solution.