Hostname: page-component-6766d58669-tq7bh Total loading time: 0 Render date: 2026-05-22T10:12:44.676Z Has data issue: false hasContentIssue false
  • English
  • Français

Miniaturization of mechanical milling for powder X-ray diffraction

Published online by Cambridge University Press:  17 August 2012

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

Abstract

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.

Keywords

grain sizeminiaturizationmicronizingmillingtungsten carbide

Information

Type
Technical Articles
Information
Powder Diffraction , Volume 27 , Issue 3 , September 2012 , pp. 189 - 193
Copyright
Copyright © International Centre for Diffraction Data 2012

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

Article purchase

Temporarily unavailable

References

Bergerioux, C., Kennedy, G. and Zikovsky, L. (1979). “Use of the semi-absolute method in neutron activation analysis”, J. Radioanal. Chem. 50, 229–234.CrossRefGoogle Scholar
Bish, D. L. and Reynolds, R. C. (1989). “Sample preparation for X-ray diffraction,” in Modern Powder Diffraction, edited by Bish, D. L. and Post, J. E. (Mineralogical Society of America, Washington), Vol. 20, pp. 73–99.CrossRefGoogle Scholar
Brandon, N. P. and Wood, R. J. K. (1993). “The influence of interfacial potential on friction and wear in an aqueous drilling mud,” Wear 170, 33–38.CrossRefGoogle Scholar
Buhrke, V. E., Jenkins, R., and Smith, D. K. (Eds.) (1998). A Practical Guide for the Preparation of Specimens for X-ray Fluorescence and X-ray Diffraction Analysis (Wiley, New York).Google Scholar
Eberl, D. D. (2003). User's guide to RockJock – A program for determining quantitative mineralogy from powder X-ray diffraction data, U.S. Geological Survey Open-File Report 2003-78, revised 2009, 47 p.Google Scholar
Heft, R. and Koszykowski, R. (1982). “Analysis of standard reference materials by absolute INAA,” J. Radioanal. Chem. 72, 245–261.CrossRefGoogle Scholar
Hickson, C. J. and Juras, S. J. (1986). “Sample contamination by grinding,” Can. Mineral. 24, 585–589.Google Scholar
Jillavenkatesa, A., Dapkunas, S. J. and Lum, L.-S. H. (2001). Particle Size Characterization. NIST Special Publication 960-1 (U.S. Government Printing Office, Washington).Google Scholar
Kleeberg, R., Monecke, T. and Hillier, S. (2008). “Preferred orientation of mineral grains in sample mounts for quantitative XRD measurements: how random are powder samples?,” Clays Clay Miner. 56, 404–415.CrossRefGoogle Scholar
Krell, A. (1995). “Load dependence of hardness in sintered submicrometer Al2O3 and ZrO2,” J. Amer. Ceram. Soc. 78, 1417–1419.CrossRefGoogle Scholar
Madsen, I. C. and Scarlett, N. V. Y. (2008). “Quantitative phase analysis,” in Powder Diffraction Theory and Practice, edited by Dinnebier, R. E. and Billinge, S. J. L. (The Royal Society of Chemistry, Cambridge), Chapter 11, pp. 298–331.CrossRefGoogle Scholar
O'Connor, B. H., Chang, W-J. (1986). “The amorphous character and particle size distribution of powders produced with the micronizing mill for quantitative X-ray powder diffractometry,” X-Ray Spec.. 15, 267–270.Google Scholar
Oerter, E. J., Brimhall, G. H. Jr., Redmond, J., and Walker, B. (2007). “A method for quantitative pyrite abundance in mine rock piles by powder X-ray diffraction and Rietveld refinement,” Appl. Geochem. 22, 2907–2925.CrossRefGoogle Scholar
Omotoso, O., McCarty, D. K., Hillier, S., and Kleeberg, R. (2006). “Some successful approaches to quantitative mineral analysis as revealed by the 3rd Reynolds Cup contest,” Clays Clay Miner., 54, 748–760.CrossRefGoogle Scholar
Quinn, G.D., Gettings, R., and Ives, L.K. (2004). “A standard reference material for Vickers hardness of ceramics and hardmetals,” in Proc. HARDMEKO 2004, Washington DC, USA, 11–12 November, 2004, 8 p.Google Scholar
Rasenack, N. and Müller, B. W. (2004). “Micron-size drug particles: common and novel micronization techniques,” Pharm. Dev. Technol. 9, 1–13.CrossRefGoogle ScholarPubMed
Raudsepp, M. and Pani, E. (2003). “Application of Rietveld analysis to environmental mineralogy,” Short Course 31, Chapter 8, pp. 165–180, Mineral. Assoc. Ottawa, Canada.Google Scholar
Smith, D. K. (1992). “Particle statistics and whole-pattern methods in quantitative X-ray powder diffraction analysis,” Adv. X-ray Anal. 35, 1–15.Google Scholar
Upadhyaya, G. S. (Ed.) (1998). Cemented Tungsten Carbides: Production, Properties, and Testing (Noyes Publications, New Jersey).Google Scholar
Van Grieken, R., Van De Velde, R. and Robberecht, H. (1980). “Sample contamination from a commercial grinding unit,” Anal. Chim. Acta 118, 137–143.CrossRefGoogle Scholar
Weitz, D. A. (2004). “Packing in the spheres,” Science 303, 968–969.CrossRefGoogle ScholarPubMed
Whitney, D. L., Broz, M. and Cook, R. F. (2007). “Hardness, toughness, and modulus of some common metamorphic minerals,” Am. Mineral. 92, 281–288.CrossRefGoogle Scholar