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通过靶向标记羧酸官能团,然后进行热解-气相色谱法分析水基聚合物体系中的酸性单体。

Acid monomer analysis in waterborne polymer systems by targeted labeling of carboxylic acid functionality, followed by pyrolysis - gas chromatography.

机构信息

DSM Coating Resins, Analytical Technology Centre, Waalwijk, The Netherlands.

DSM Coating Resins, Analytical Technology Centre, Waalwijk, The Netherlands.

出版信息

J Chromatogr A. 2018 Jul 27;1560:63-70. doi: 10.1016/j.chroma.2018.05.024. Epub 2018 May 14.

Abstract

Pyrolysis - gas chromatography - (PyGC) is a common method to analyse the composition of natural and synthetic resins. The analysis of acid functionality in, for example, waterborne polyacrylates and polyurethanes polymers has proven to be difficult due to solubility issues, inter- and intramolecular interaction effects, lack of detectability in chromatographic analysis, and lack of thermal stability. Conventional analytical techniques, such as PyGC, cannot be used for the direct detection and identification of acidic monomers, due to thermal rearrangements that take place during pyrolysis. To circumvent this, the carboxylic acid groups are protected prior to thermal treatment by reaction with 2-bromoacetophenone. Reaction conditions are investigated and optimised wrt. conversion measurements. The aproach is applied to waterborne polyacryalates and the results are discussed. This approach enables identification and (semi)quantitative analysis of different acid functionalities in waterborne polymers by PyGC.

摘要

热解气相色谱法(PyGC)是一种分析天然和合成树脂组成的常用方法。由于溶解度问题、分子内和分子间相互作用效应、色谱分析中的检测性差以及热稳定性差,分析例如水性聚丙烯酸酯和聚氨酯聚合物中的酸官能团已被证明是困难的。由于热解过程中发生的热重排,常规分析技术(如 PyGC)不能用于直接检测和识别酸性单体。为了克服这个问题,在热处理之前,通过与 2-溴苯乙酮反应将羧酸基团保护起来。反应条件进行了研究和优化,以测量转化率。该方法应用于水性聚丙烯酸酯,并对结果进行了讨论。该方法通过 PyGC 实现了对水性聚合物中不同酸官能团的鉴定和(半)定量分析。

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