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Miniaturization of mechanical milling for powder X-ray diffraction

Published online by Cambridge University Press:  17 August 2012

Andrew J. Locock*
Department of Earth and Atmospheric Sciences, University of Alberta, Edmonton, Alberta T6G 2E3, Canada
David Chesterman
Department of Earth and Atmospheric Sciences, University of Alberta, Edmonton, Alberta T6G 2E3, Canada
Diane Caird
Department of Earth and Atmospheric Sciences, University of Alberta, Edmonton, Alberta T6G 2E3, Canada
M. John M. Duke
SLOWPOKE Nuclear Reactor Facility, University of Alberta, Edmonton, Alberta T6G 2N8, Canada
a)Author to whom correspondence should be addressed. Electronic mail:


To enable mechanical milling of small (0.1–1.0 g) samples, a cylindrical grinding vessel machined from polypropylene and furnished with tungsten carbide rods has been designed and produced for use inside the conventional jar of a McCrone Micronizing Mill. The vessel is about one-seventh the volume of the conventional jar supplied by the manufacturer. The conditions of milling for both the conventional and the miniaturized-grinding assemblies were tested using quartz sand as a limiting case. The median grain sizes of the resultant powders were measured by an X-ray gravitational-sedimentation method, with contamination from the grinding media measured by Rietveld refinement and by instrumental neutron activation analysis. The use of tungsten carbide grinding elements permits rapid wet milling of a small sample to the same median grain size in about one-third of the time required by a regular sample ground in corundum. The relative contamination (by tungsten carbide on a weight basis) using the miniaturized-grinding assembly is about 6(1)% of the proportion of corundum contamination yielded by the conventional grinding assembly.

Technical Articles
Copyright © International Centre for Diffraction Data 2012

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