A novel analytical pyrolysis device applicable for measurements of less volatile pyrolyzates

作者:Kano Hirohisa; Okamoto Takahiro; Kitagawa Shinya; Iiguni Yoshinori; Ohtani Hajime*; Ito Hiroshi; Iwai Koichiro; Kuno Minoru
来源:Journal of Analytical and Applied Pyrolysis, 2015, 113: 165-173.
DOI:10.1016/j.jaap.2014.12.008

摘要

A novel analytical pyrolysis device suitable for the measurements of the less volatile pyrolyzates was developed. This device is comprised of a pyrolysis unit based on the vertical microfurnace pyrolyzer and a movable pyrolysis tube made of stainless steel. The upper side of the pyrolysis tube is first set at the heated center of the pyrolysis unit. A polymer sample in a sample cup is introduced into the heated center and pyrolyzed under the flow of nitrogen carrier gas. The pyrolyzates are then transferred to the bottom side of the pyrolysis tube which is cooled down by air blow and the less volatile pyrolyzates are condensed. After that the pyrolysis tube is moved down out of the pyrolysis unit and blocked from the hot zone by moving the three port valve. Finally the trapped pyrolyzates are flushed by an appropriate solvent into a collection vial. The recovered pyrolyzates in the solution can be then subjected to the measurements suitable for less volatile products such as matrix-assisted laser desorption/ionization mass spectrometry. Moreover, this device is also on-line connected to the injection port of a high performance liquid chromatographic system, which is also appropriate for the measurements of oligomeric products. The basic performance of the developed device was tested by using some polymer samples forming less volatile pyrolyzates such as poly(butylene terephthalate) and poly(2,6-dimethy1-1,4-phenylene ether). In addition, the usefulness of this method was demonstrated through the characterization of the crosslinking sequences in a photocured resin combined with the thermally-assisted hydrolysis and methylation reaction.

  • 出版日期2015-5