A novel analytical pyrolysis device applicable for measurements of less volatile pyrolyzates
A novel analytical pyrolysis device applicable for measurements of less volatile pyrolyzates
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DOI：
10.1016/j.jaap.2014.12.008
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发表时间：
2015-05
影响因子：
6
通讯作者：
Hirohisa Kano;Takahiro Okamoto;S. Kitagawa;Yoshinori Iiguni;H. Ohtani;Hiroshi Ito;Koichiro Iwai;M. Kuno
中科院分区：
文献类型：
--
作者：
Hirohisa Kano;Takahiro Okamoto;S. Kitagawa;Yoshinori Iiguni;H. Ohtani;Hiroshi Ito;Koichiro Iwai;M. Kuno
开发了一种适合测量不易挥发的热解产物的新型分析热解装置。该装置由基于立式微型炉热解炉的热解装置和不锈钢制成的可移动热解管组成。首先将热解管的上侧设置在热解单元的受热中心。将样品杯中的聚合物样品引入加热中心并在氮气载气流下热解。然后将热解产物转移到热解管的底部，通过鼓风将其冷却，并且将不易挥发的热解产物冷凝。之后，将热解管向下移出热解装置，并通过移动三通阀将其与热区隔开。最后，用适当的溶剂将捕获的热解产物冲入收集瓶中。然后可以对溶液中回收的热解产物进行适合于挥发性较小的产品的测量，例如基质辅助激光解吸/电离质谱法。此外，该装置还在线连接至高效液相色谱系统的进样口，这也适用于低聚产物的测量。通过使用一些形成不易挥发的热解产物的聚合物样品（例如聚对苯二甲酸丁二醇酯和聚2,6-二甲基-1,4-苯醚）来测试所开发的装置的基本性能。此外，通过光固化树脂中交联序列的表征以及热辅助水解和甲基化反应，证明了该方法的实用性。
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-dimethyl-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.