Microporous carbons characterized by different structural properties w
ere prepared by carbonization of poly(sodium-4-styrenesulfonate) in a
nitrogen flow at temperatures in the range of 500-850 degrees C. The c
arbonization process and the microstructural characteristics of the ca
rbonaceous materials obtained have been studied by differential therma
l analysis (DTA); diffuse reflectance FT-IR spectroscopy, inverse gas
chromatography at infinite dilution (IGC), and sorption experiments. T
he temperature controlled carbonization of poly(sodium-4-styrenesulfon
ate) leads, in one step, to formation of microporous carbons without u
sing additional activation procedures. The pore sizes of the materials
obtained were limited to the range of 0.38-0.6 nm, with wider, and th
us more heterogeneous, micropore size distributions at higher temperat
ure of heat treatment. The conclusions obtained are derived from adsor
ption studies of methane under conditions when monolayer adsorption is
dominant and thus direct information of adsorbate/adsorbent interacti
ons as a function of microstructural changes during carbonization can
be revealed. Consistency is found with data from the other techniques
employed.