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In situ monitoring of powder reactions in percolating solution by wet‐cell X‐ray diffraction techniques
Author(s) -
Warr Laurence N.,
Hofmann Heiko
Publication year - 2003
Publication title -
journal of applied crystallography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.429
H-Index - 162
ISSN - 1600-5767
DOI - 10.1107/s0021889803004333
Subject(s) - dissolution , powder diffraction , crystallization , diffractometer , powder diffractometer , diffraction , in situ , kinetics , materials science , crystal (programming language) , chemical reaction , analytical chemistry (journal) , chemical engineering , x ray crystallography , chemistry , crystallography , crystal structure , chromatography , optics , organic chemistry , programming language , physics , quantum mechanics , computer science , engineering
This note describes how the kinetics of powder reactions in percolating solution can be studied by X‐ray diffraction using a wet‐cell flow‐through reaction chamber. The device can be routinely moved between diffractometer and controlled laboratory (pressure, temperature) conditions with the ease of a standard powder holder. Short‐term in situ measurements and long‐term quasi in situ monitoring of dissolution and crystallization reactions are possible with a minimum of sample preparation and little disturbance of the system. Measuring time‐dependent changes in the concentration of crystalline reactants and products provides information for quantifying reaction kinetics and for determining dissolution and crystal growth mechanisms. Results can be compared with changes in solution chemistry of the collected eluate, enabling a more complete reconstruction of heterogeneous crystal–solution reactions in open systems.