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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