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

Journal of chromatography. A (2018-05-19)
T Brooijmans, R Okhuijsen, I Oerlemans, P J Schoenmakers, R Peters
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.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Propyl chloroformate, 98%
Sigma-Aldrich
2-Bromo-4′-nitroacetophenone, 95%
Sigma-Aldrich
6-Benzylaminopurine hydrochloride, suitable for plant cell culture, ≥98%