A flow-through reaction cell that couples time-resolved X-ray diffraction with stable isotope analysis

A non-metallic flow-through reaction cell is described, designed forin situtime-resolved X-ray diffraction coupled with stable isotope analysis. The experimental setup allows the correlation of Cu isotope fractionation with changes in crystal structure during copper sulfide dissolution. This flow-through cell can be applied to many classes of fluid–mineral reactions that involve dissolution or ion exchange.

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A Flow-Through Reaction Cell for Studying Minerals Leaching by In-Situ Synchrotron Powder X-ray Diffraction

Minerals ◽

10.3390/min10110990 ◽

2020 ◽

Vol 10 (11) ◽

pp. 990

Author(s):

Fatemeh Nikkhou ◽

Fang Xia ◽

Xizhi Yao ◽

Idowu A. Adegoke ◽

Qinfen Gu ◽

...

Keyword(s):

Flow Rate ◽

Pressure Leaching ◽

X Ray Diffraction ◽

Reaction Cell ◽

Time Resolved ◽

X Ray ◽

Ore Minerals ◽

Flow Through ◽

Diffraction Patterns

A flow-through reaction cell has been developed for studying minerals leaching by in-situ time-resolved powder X-ray diffraction, allowing for a better understanding of the leaching mechanisms and kinetics. The cell has the capability of independent control of temperature (up to 95 °C) and flow rate (>0.5 mL min−1) for atmospheric pressure leaching. It was successfully tested at the powder diffraction beamline at the Australian Synchrotron. Galena powder was leached in a citrate solution under flow-through condition at a flow rate of 0.5 mL min−1, while diffraction patterns were collected during the entire leaching process, showing rapid galena dissolution without the formation of secondary mineral phases. The flow-through cell can be used to study leaching processes of other ore minerals.

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A reaction cell for time-resolvedin situXAS studies during wet chemical synthesis: the Cu2(OH)3Cl case

Journal of Synchrotron Radiation ◽

10.1107/s1600577513028786 ◽

2013 ◽

Vol 21 (1) ◽

pp. 254-258 ◽

Cited By ~ 9

Author(s):

Jocenir Boita ◽

Maria do Carmo Martins Alves ◽

Jonder Morais

Keyword(s):

Chemical Synthesis ◽

Photoelectron Spectroscopy ◽

X Ray Diffraction ◽

Reaction Cell ◽

Time Resolved ◽

X Ray ◽

Wet Chemical Synthesis ◽

X Ray Absorption ◽

Electronic And Structural Properties

The use ofin situtime-resolved dispersive X-ray absorption spectroscopy (DXAS) to monitor the formation of Cu2(OH)3Cl particles in an aqueous solution is reported. The measurements were performed using a dedicated reaction cell, which enabled the evolution of the CuK-edge X-ray absorption near-edge spectroscopy to be followed during mild chemical synthesis. The formed Cu2(OH)3Cl particles were also characterized by synchrotron-radiation-excited X-ray photoelectron spectroscopy, X-ray diffraction and scanning electron microscopy. The influence of polyvinylpyrrolidone (PVP) on the electronic and structural properties of the formed particles was investigated. The results indicate clearly the formation of Cu2(OH)3Cl, with or without the use of PVP, which presents very similar crystalline structures in the long-range order. However, depending on the reaction, dramatic differences were observed byin situDXAS in the vicinities of the Cu atoms.

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Development of an In-Situ Mass Spectrometer for Stable Isotope Analysis

10.21236/ada620413 ◽

2003 ◽

Author(s):

R. T. Short ◽

Gottfried P. Kibelka ◽

Robert H. Byrne ◽

David Hollander

Keyword(s):

Stable Isotope ◽

Mass Spectrometer ◽

Stable Isotope Analysis ◽

Isotope Analysis

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In situ time resolved wide angle X-ray diffraction study of nanotube carpet growth: Nature of catalyst particles and progressive nanotube alignment

Carbon ◽

10.1016/j.carbon.2015.01.046 ◽

2015 ◽

Vol 87 ◽

pp. 246-256 ◽

Cited By ~ 10

Author(s):

Périne Landois ◽

Mathieu Pinault ◽

Stéphan Rouzière ◽

Dominique Porterat ◽

Cristian Mocuta ◽

...

Keyword(s):

Diffraction Study ◽

Wide Angle ◽

X Ray Diffraction ◽

Time Resolved ◽

X Ray

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Electric-field-induced lattice distortion in epitaxial BiFeO3 thin films as determined by in situ time-resolved x-ray diffraction

Applied Physics Letters ◽

10.1063/1.5000495 ◽

2017 ◽

Vol 111 (8) ◽

pp. 082907 ◽

Cited By ~ 2

Author(s):

Seiji Nakashima ◽

Osami Sakata ◽

Hiroshi Funakubo ◽

Takao Shimizu ◽

Daichi Ichinose ◽

...

Keyword(s):

Thin Films ◽

Electric Field ◽

Lattice Distortion ◽

X Ray Diffraction ◽

Time Resolved ◽

X Ray ◽

Bifeo3 Thin Films

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Green rust as a precursor for magnetite: an in situ synchrotron based study

Mineralogical Magazine ◽

10.1180/minmag.2008.072.1.201 ◽

2008 ◽

Vol 72 (1) ◽

pp. 201-204 ◽

Cited By ~ 40

Author(s):

A. Sumoondur ◽

S. Shaw ◽

I. Ahmed ◽

L. G. Benning

Keyword(s):

Direct Evidence ◽

Green Rust ◽

Stable Phase ◽

X Ray Diffraction ◽

Time Resolved ◽

X Ray ◽

Subsequent Transformation ◽

Rapid Formation ◽

Reaction Proceeds

AbstractIn this study, direct evidence for the formation of magnetite via a green rust intermediate is reported. The Fe(II) induced transformation of ferrihydrite, was quantified in situ and under O2-free conditions using synchrotron-based time-resolved energy dispersive X-ray diffraction. At pH 9 and Fe(II)/Fe(III) ratios of 0.5 and 1, rapid growth (6 min) of sulphate green rust and its subsequent transformation to magnetite was observed. Electron microscopy confirmed these results, showing the initial rapid formation of hexagonal sulphate green rust particles, followed by the corrosion of the green rust as magnetite growth occurred, indicating that the reaction proceeds via a dissolution-reprecipitation mechanism. At pH 7 and Fe(II)/Fe(III) ratio of 0.5, sulphate green rust was the stable phase, with no transformation to magnetite.

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Time-resolved, in situ X-ray diffraction studies of the hydrothermal syntheses of microporous materials

Microporous and Mesoporous Materials ◽

10.1016/s1387-1811(98)00009-2 ◽

1998 ◽

Vol 21 (4-6) ◽

pp. 253-262 ◽

Cited By ~ 19

Author(s):

Dermot O'Hare ◽

John S.O. Evans ◽

Robin J. Francis ◽

P. Shiv Halasyamani ◽

Poul Norby ◽

...

Keyword(s):

Microporous Materials ◽

X Ray Diffraction ◽

Time Resolved ◽

X Ray ◽

Hydrothermal Syntheses

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Elucidating the Structural Evolution of a Highy Porous Responsive Metal-Organic Framework (DUT-49(M)) upon Guests Desorption by Time-Resolved In-Situ Powder X-Ray Diffraction

10.26434/chemrxiv.12753593.v1 ◽

2020 ◽

Author(s):

Bikash Garai ◽

Volodymyr Bon ◽

Francesco Walenszus ◽

Azat Khadiev ◽

Dmitri Novikov ◽

...

Keyword(s):

Adsorption Isotherms ◽

Metal Organic Framework ◽

Structural Evolution ◽

Structural Transformations ◽

X Ray Diffraction ◽

Time Resolved ◽

X Ray ◽

Metal Organic ◽

Subcritical Fluid

Variation in the metal centres of M-M paddle-wheel SBU results in the formation of isostructural DUT-49(M) frameworks. However, the porosity of the framework was found to be different for each of the structures. While a high and moderate porosity was obtained for DUT-49(Cu) and DUT-49(Ni), respectively, other members of the series [DUT-49(M); M= Mn, Fe, Co, Zn, Cd] show very low porosity and shapes of the adsorption isotherms which is not expected for op phases of these MOFs. Investigation on those MOFs revealed that those frameworks undergo structural collapse during the solvent removal at the activation step. Thus, herein, we aimed to study the detailed structural transformations that are possibly occurring during the removal of the subcritical fluid from the framework.

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Time-resolved XRD experiments for a fine description of mechanisms induced during reactive sintering

Science of Sintering ◽

10.2298/sos0501027p ◽

2005 ◽

Vol 37 (1) ◽

pp. 27-34 ◽

Cited By ~ 7

Author(s):

S. Paris ◽

E. Gaffet ◽

D. Vrel ◽

D. Thiaudiere ◽

M. Gailhanou ◽

...

Keyword(s):

Reactive Sintering ◽

X Ray Diffraction ◽

Reaction Parameters ◽

Time Resolved ◽

X Ray ◽

Synthesis Conditions ◽

Nanostructure Materials ◽

Synchrotron Beam ◽

The One

The control of Mechanically Activated Field Activated Pressure Assisted Synthesis hereafter called the MAFAPAS process is the main objective to be achieved for producing nanostructure materials with a controlled consolidation level. Consequently, it was essential to develop characterization tools "in situ" such as the Time Resolved X-ray Diffraction (TRXRD), with an X-ray synchrotron beam (H10, LURE Orsay) coupled to an infrared thermography to study simultaneously structural transformations and thermal evolutions. From the 2003 experiments, we took the opportunity to modify the sample-holder in order to reproduce the better synthesis conditions of the MAFAPAS process, but without the consolidation step. The versatility of the setup has been proved and could even be enhanced by the design of new sample holders. In addition, this work clearly shows that this equipment will allow, on the one hand, to make progress of the understanding of MAFAPAS mechanisms and, on the other hand, to adjust reaction parameters (mechanical activation and combustion synthesis) for producing many materials with an expected microstructure.

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