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The quantitative phase analysis of clay minerals by X-ray diffraction: modern aspects of industrial routine control

Published online by Cambridge University Press:  09 July 2018

D. Minichelli
D. Minichelli*
Affiliation:
Ceramica Fine S.p.A., Sassuolo, Modena, Italy
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Abstract

The method described uses external standard mixtures, both natural and artificial. Variations in degree of structural order between standard and analyte mineral are taken into account. ‘Amorphous’ materials in standard mixtures are simulated by alkali-boron-silicon glasses. Variations in response of the X-ray equipment with time are assessed by running a standard multiphase mixture. Strict control is exercised on particle orientation, and thermal treatments are used to separate overlapping reflections in the low-2θ region.

Resume

Resume

On décrit les résultats d'une recherche ayant pour but d'explorer les limites et les possibilités de la détermination quantitative par diffraction de rayons X de poudre pour des aggrégats complexes tel que les shistes et les minéraux argileux. On utilise la largeur à mi-hauteur des pics de diffraction pour calibrer les intensités intégrées. Le contrôle de la réponse électronique de l'équipement des rayons X est effectué en vue d'une calibration absolue des courbes analytiques par une méthode de moindre carré. Un contrôle strict de la forme des échantillons ainsi que le traitement thermique des poudres est utilisé pour obtenir de bons résultats en vue de séparer les réflexions qui se supperposent dans la zone des faibles valeurs de 2θ.

Kurzreferat

Kurzreferat

Zur quantitativen Phasenanalyse wird ein Verfahren beschrieben, für das sowohl synthetische als auch natürliche Standardproben verwendet werden. Unterschiede in der Kristallinität zwischen Standard- und Analysenmaterial werden berücksichtigt. Zur Simulation von ‘amorphem’ Material werden Alkali-Borosilicatgläser verwendet. Zeitliche Variationen des Meßsignals werden durch Zwischenschaltung von Multiphasen-Standards erfaßt. Besondere Beachtung wird auf eine konstante Orientierung der Partikel gelegt; Überlappungen im Kleinwinkelbereich werden durch thermische Behandlung der Proben ausgeschaltet.

Resumen

Resumen

El método utiliza mezclas externas standard, naturales y artificiales. Se tienen en cuenta las variaciones del grado de orden estructural entre los standards y los minerales a analizar. Los materiales ‘amorfos’, en las mezclas standard, son simulados con vidrios de borosilicatos alcalinos. Las variaciones en la respuesta del equipo de rayos X con el tiempo, son calculadas previamente utilizando una mezcla standard multifase. Se controla estrictamente el grado de orientación de las partículas, y para separar reflexiones superpuestas en la zona de pequeños ángulos, se usan tratamientos térmicos.

Type
Research Article
Information
Clay Minerals , Volume 17 , Issue 4 , December 1982 , pp. 401 - 408
Copyright
Copyright © The Mineralogical Society of Great Britain and Ireland 1982

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