Distribution analysis of functional groups in polymers by derivatization-electron probe X-ray microanalysis

摘要

A new analytical method referred to as derivatization-electron probe X-ray microanalysis (XMA) has been developed to deter- mine the distribution of 0.1/100 order functional groups in polymers with pm level lateral resolution. The fundamental performance of XMA in analyzing derivatized polymers has been investigated. The results showed that the detection limit for the concentration of Br in a brominated epoxy resin was 0.05/100 and the lateral resolution was 3 μm. Also, the optimal reaction conditions that make it possible to derivatize selectively the vinyl groups, the carboxyl groups and the carbonyl groups have been found. These conditions are the key to this method. In addition, the depth profile of the vinyl groups in amine-degraded poly (vinyl chloride) has been analyzed using this method. Since the depth profiles agreed well with those obtained by micro-IR spectroscopy, the reliability of the distribution measurement of functional groups by this method was confirmed. 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 ethylene-carbon monoxide copolymer have proved that this method is useful for the characterization of polymers and the study of polymer degradation.