Vol.34 No.1(1999.3)
Research Report

Distribution Analysis of Functional Groups in Polymers by Derivatization-Electron Probe X-ray Microanalysis ( EPMA )
Motoyasu Sugiura, Atsushi Murase,
Keiko Fukumoto, Takuya Mitsuoka,
Masao Tsuji

The new analytic method referred to as gDerivatization-Electron probe X-ray microanalysis (EPMA)hhas been developed to determine the distribution of 0.1% order functional groups in polymers with μm level lateral resolution.
This method first derivatizes a functional group using a reaction reagent with indicator elements highly sensitive to EPMA and then measures the distribution of the indicator elements, thus obtaining the distribution of the original functional group.

Fundamental performances of EPMA in analyzing derivatized polymers have been investigated. The results showed that the detection limit for the concentration of Br in the brominated epoxy resin was 0.05% and the lateral resolution was 3μm.

Also, the optimal reaction condition that makes it possible to derivatize the C = C bonds and the COOH bonds selectively has been found. This condition is the key of this method.

In addition, the depth distribution of C = C bonds in amine-degraded polyvinyl chloride has been analyzed using this method. The results agreed well with those obtained by micro-IR spectroscopy. By this method, the sensitivity was 30 times higher, and the lateral resolution was 4 times higher than those obtained by the micro-IR spectroscopy.
The actual applications to the depth analysis of degraded Nylon-6 and polyethyrene have proved that this method is useful for the characterization of polymers and studies on polymer degradation.
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