Nano powder of natural clinoptilolite zeolite was mechanically prepared by using a planetary ball mill. Statistical experimental design was applied to optimize wet and dry milling of clinoptilolite zeolite. To determine appropriate milling conditions with respect to the final product crystallinity, particle size and distribution, different milling parameters such as dry and wet milling durations, rotational speed, balls to powder ratio and water to powder ratio (for the wet milling) were investigated. Laser beam scattering technique, scanning electron microscopy and X-ray diffraction analyses were carried out to characterize samples. Results showed that larger than 1 mm particle size of clinoptilolite powder may mechanically be reduced into the size range of less than 100 nm to 30 mu m by means of planetary ball milling. (C) 2010 Elsevier B.V. All rights reserved.