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TG-EGA Systems |
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TG-EGA Systems (Evolved
Gas Analysis, MS and/or FTIR) / Problems related to the
identification of thermal decomposition of solids
Solid state kinetic analysis can be also used for the
elaboration of the results obtained by hyphenated techniques
such as TG-MS or TG-FTIR. The application of these techniques is
widely recognized for the characterization of the degradation of
solids [1].
One of the problems related to the measurement and analysis of
material decomposition is the time lag observed between:
- the DTG- (or TG) signal due to the decomposition of the solids
and
- the MS or FTIR signal of
the evolving gas (EGA signals).
In order to apply correctly the EGA signals for the description
of the kinetics of the decomposition of solids, the
interrelation between thermoanalytical and mass spectrometric
curves in the TA-MS and/or TA-FTIR system has to be known. The
proper description of the input signal DTG by the output signal
(EGA) depends on the convective and diffusional mass transfer
occurring in combined thermoanalyzer-EGA systems [2]. More
generally, the difference between input and output signals
depends on:
- the carrier gas flow rate (residence time in the
thermoanalyzer chamber and distance between thermoanalyzer and
EGA system)
- the back-mixing of the carrier gas in the thermoanalyzer
chamber (mixed-flow volume and plug-flow volume)
- the choice of the carrier gas (the diffusion of the
evolved gas in the carrier gas)
- the temperature (non-isothermal experiments progressively
modify the diffusion of the evolved gas in the carrier gas)
[1] K.G.H. Raemaekers, J.C.J. Bart, Thermochim. Acta, 295 (1997)
1.
[2] B. Roduit, J. Baldyga, M. Maciejewski and A. Baiker,
Thermochim. Acta, 295 (1997) 59.
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