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Clay Minerals; September 2002; v. 37; no. 3; p. 487-496; DOI: 10.1180/0009855023730047
© 2002 Mineralogical Society of Great Britain and Ireland
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Research Paper

Identification of halloysite (7 Å) by ethylene glycol solvation: the ‘MacEwan effect’

S. HILLIER1,* and P. C. RYAN2

1 Macaulay Institute, Craigiebuckler, Aberdeen, AB15 8QH, UK, and 2 Geology Department, Middlebury College, Middlebury, VT 05753 USA

* E-mail: s.hillier{at}macaulay.ac.uk

(Received 14 September 2001; revised 14 January 2002)

X-ray powder diffraction patterns of halloysite (7 Å) are characteristically altered following solvation with ethylene glycol. Some effect was first noted in the classic work of MacEwan but its value in the unequivocal identification of halloysite (7 Å) seems to have been overlooked subsequently. The response to ethylene glycol solvation involves a decrease in the intensity (peak height) of the peak at ~7.2 Å and an increase in the intensity (peak height) of the peak at ~3.58 Å thus narrowing the 7.2 Å/3.58 Å peak height intensity ratio. For pure samples of halloysite, this ratio is narrowed by an average of ~50%. This distinctive change is related to the interstratified nature of halloysite (7 Å), specifically the presence of ‘residual’ interlayer water, i.e. halloysite (10 Å), which can be replaced with ethylene glycol so forming 10.9 Å layers, a spacing that is almost exactly one and a half times the thickness of dehydrated (7.2 Å) layers which do not imbibe ethylene glycol. Thus the separation between the 001 peaks in the 7.2 Å/10.9 Å interstratification is increased and the 0027.2 (3.58 Å) and 00310.9 (3.63 Å) peaks become more or less coincident, compared to the 7.2 Å/10 Å interstratification, i.e. the partially hydrated state. The widespread use of ethylene glycol solvation in clay mineral studies makes it a particularly useful and simple test to determine the presence of halloysite. Pure halloysites should be readily identifiable and experiments indicate a ‘routine’ sensitivity of ~20% halloysite in mixtures with kaolinite, although this will depend on factors such as ‘crystallinity’ and could be improved with careful attention to intensity measurements. It is proposed to call this phenomenon the ‘MacEwan effect’ in honour of its discoverer Douglas Maclean Clark MacEwan.

KEYWORDS: halloysite, kaolinite, kaolin, ethylene glycol, X-ray powder diffraction, MacEwan




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