M. Stenseng et al., Investigation of biomass pyrolysis by thermogravimetric analysis and differential scanning calorimetry, J AN AP PYR, 58, 2001, pp. 765-780
The influence of sample size on the pyrolysis of wheat straw and three type
s of cellulose has been investigated by simultaneous thermogravimetric anal
ysis and differential scanning calorimetry. Samples between 2 and 20 mg wer
e pyrolyzed to a maximum temperature of 600 degreesC at a heating rate of 4
0 degreesC min(-1). It was found that sample size had a large effect on the
pyrolysis of Avicel cellulose; the mass loss peak was shifted to higher te
mperatures at higher sample mass. However, the effect of sample mass on the
pyrolysis of wheat straw was insignificant. In wheat straw samples washed
in water to reduce the KCl content, the influence of sample size was betwee
n that of cellulose and straw, but closer to straw. A model for the TGA/DSC
-system has been developed, which includes heat transfer by both convection
and radiation to the two crucibles and the sample. Simulations with the mo
del showed that the sample mass had a large influence on the pyrolysis at h
igh heat of reaction and in agreement with data, the pyrolysis peak shifts
to higher temperatures at higher sample mass. The recommendation found in t
he literature that samples should be no larger than 1 mg in TGA measurement
s must be limited to biomass samples with a high heat of reaction such as c
ellulose. (C) 2001 Elsevier Science B.V. All rights reserved.