G. Delapuente et al., THERMAL-STABILITY OF OXYGENATED FUNCTIONS IN ACTIVATED CARBONS, Journal of analytical and applied pyrolysis, 43(2), 1997, pp. 125-138
Activated carbons with various degrees of oxidation were prepared by t
reatment with concentrated nitric acid at various temperatures. Select
ive removal of the oxygen complexes by heating under nitrogen flow at
573, 773 and 1073 K was also considered. The samples were characterise
d through temperature-programmed desorption (TPD), Fourier transformed
infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XP
S) techniques, FTIR and XPS techniques were found to be very useful fo
r relating the shape of CO2 desorption profiles during pyrolysis with
the nature of the functional groups desorbed. Three steps in TPD profi
les were observed: (i) the desorption of carboxylic acid groups in the
form of CO2 in the lower temperature range, 400-623 K; (ii) the decom
position of lactone groups created during HNO3 treatment and, to some
extent, originated during heating rearrangements, in the temperature r
ange 623-823 K; and (iii) the elimination of the more stable ether gro
ups upon treatment at temperatures above 823 K. The combination of the
se three techniques (TPD, FTIR and XPS) gives a reasonable picture of
the surface chemistry of the oxidised activated carbons. (C) 1997 Else
vier Science B.V.