Experimental procedures used at the preparation and characterization stages of nanoporous materials (NPM) from 1,2-polybutadiene-b-polydimethylsiloxane (1,2-PB-b-PDMS) block copolymers are presented. The NPM were obtained from self-assembled block copolymers after firstly cross-linking 1,2-PB (the matrix component) and secondly degrading PDMS (the expendable component). Depending on the temperature of the cross-linking reaction different morphologies can be 'frozen' from the same block copolymer. Starting with a block copolymer precursor of lamellar morphology at room temperature, the gyroid structure or a metastable structure showing hexagonal symmetry (probably HPL) were permanently captured by cross-linking the precursor at 140 degrees C or at 85 degrees C, respectively. PDMS was degraded by reaction with tetrabutylamonium fluoride; considerations on the mechanism of cleaving reaction are presented. The characterization of the materials at different stages of preparation includes gravimetry, infrared spectroscopy, small angle x-ray scattering, electron microscopy and isothermal nitrogen adsorption experiments. (C) 2010 Elsevier Ltd. All rights reserved.