Supported carbon molecular sieve membranes (CMSMs) were prepared by the pyr
olysis of a polyetherimide (PEI) polymeric precursor The membranes were cha
racterized by scanning electron microscopy, energy dispersive spectroscopy,
and micropore analysis, using gas adsorption techniques to relate their mi
crostructure characteristics to their transport and separation characterist
ics. The analysis shows that preparation conditions determine whether the c
arbon molecular sieve layer forms within or outside the gamma -alumina laye
r of the substrate. Micropore CO2 and N-2 adsorption analysis of both suppo
rted and unsupported CMSMS showed a sharp peak at about (3.6-3.8) x 10(-10)
m using the Horvath-Kawazoe method For the supported CMSMs it was observed
that consecutive coating/carbonization steps reduced the pore volume in th
e micro- and mesoporous regions, without greatly affecting the volume of po
res in the range of (3.5-6) x 10(-10) m. The reduction of the pore volume i
n the micro- and mesoporous regions is accompanied by an increase in the se
paration factor and a decrease in the permeance after each coating/carboniz
ation cycle. Micropore analysis of a membrane, whose performance had degrad
ed, indicated that its volume of pores between (3.6-6) x 10(-10) m had dras
tically decreased from the corresponding value of the as-prepared membranes
.