Startseite Quantification of minor phases in growth kinetics experiments with powder X-ray diffraction
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Quantification of minor phases in growth kinetics experiments with powder X-ray diffraction

  • John M. Hanchar , Kathryn L. Nagy , Paul Fenter , Robert J. Finch , Donald J. Beno und Neil C. Sturchio EMAIL logo
Veröffentlicht/Copyright: 25. März 2015
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Abstract

Minor amounts of clay minerals precipitated from aqueous solution can be rapidly identified and quantified in a mineral mixture with powder X-ray diffraction using a rotating-anode source and a position-sensitive detector. For the case of gibbsite precipitated on a kaolinite powder substrate we demonstrate a simple method having a minimum detection limit of 0.1 wt%, using pure gibbsite as the intensity reference in mechanical mixtures of gibbsite and kaolinite. The amount of gibbsite precipitated onto kaolinite at 80 °C, pH 3 is higher when determined from solution chemistry than from the X-ray method, and the difference in amounts increases with increasing Al concentration in solution. This discrepancy can be explained by assuming that a fraction of the precipitated material is effectively invisible to the X-ray diffraction technique, either due to a small diffracting domain size along the gibbsite [001] direction or formation of an Al-phase that is amorphous to X-rays. This method should be generally useful for a range of mineral mixtures where at least one intense reflection for the phase of interest is not obscured. The ability to identify, characterize, and quantify trace phases by X-ray diffraction, especially when combined with surface analysis by electron or atomic force imaging, is an important complement to the conventional approach of monitoring solution composition in growth kinetics experiments.

Received: 1998-12-22
Accepted: 2000-4-6
Published Online: 2015-3-25
Published in Print: 2000-8-1

© 2015 by Walter de Gruyter Berlin/Boston

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