Abstract
A coiled-filament probe of a commercially available pyrolyzer (Chemical Data Systems, CDS Pyroprobe 120) was modified to change the temporal and spatial temperature profiles delivered by the probe. The modification changes the geometry of the heating filament: it is coiled tightly and a light coating of a ceramic cement is applied to maintain its dimensional stability while minimizing the possibility of developing an electrical short. The modified pyroprobe produced a reproducible and uniform temperature profile over a ∼3-mm long pyrolysis region and had near-perfect emissivity (∼0.95) for monitoring temperature with an optical thermometer. To conduct experiments off-line we also designed a glass housing for the tightly-coiled pyroprobe (TC-pyp). The housing has provisions for making a gas-tight seal with the pyroprobe, for introducing a gas to control the pyrolysis atmosphere and provide a rapid sweep of the pyrolysis region and for interfacing with a pre-trap to collect pyrolysates. To evaluate the results obtained with the TC-pyp we compared mass and temperature dependencies of Kraton D1107P pyrograms with those generated by a Pt ribbon-pyroprobe (PtR-pyp) and an unmodified coil pyroprobe. In addition, we report on the use of the instrumentation for quantitative analyses of model polymers.
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