Ten montmorillonite-type clay samples from Miles, Queensland, Australia, have been characterised using XRD, ICP-AES and infrared spectroscopy. The Na-exchanged sample, DH-30, was used for pillaring with Al-13 by exchange with an Al(NO3)(3)/NaOH solution with an approximate OH/Al molar ratio of 2.2. The XRD pattern for the expanded smectite provided evidence that the Na/Al-13 polymer exchange had occurred. XRD patterns for the raw sample, the Na-exchanged clay and the Al-13-exchanged clay resulted in d-spacings of 15.09, 15.73 and 17.42 Angstrom, respectively. Calcination at 600 degreesC of the Al-13-smectite led to a minor decrease in basal spacing to approximately 16.5 Angstrom. The effect of temperature on the Al-13-expanded smectite was also apparent when the d-spacing of an air-dried sample (19.44 Angstrom) was compared to that of an oven-dried (60 degreesC) sample (17.42 Angstrom). This difference was due to the loss of water molecules from the Al-13 outer sphere of hydration. (C) 2002 Elsevier Science B.V. All rights reserved.